CO2 Production Rate Research Articles

Recyclable porous core-shell Mn-Co-O flame retardant for improving flame retardancy and smoke suppression of epoxy resin

The development of metal oxide flame retardants that are easy to synthesize, efficient, and recyclable would be more beneficial to circular economy. In this work, a porous core-shell Mn3CoOx was developed to efficiently reduce heat, smoke as well as hazardous gas during the combustion of epoxy resin (EP). Compared with pure EP, the peak heat release rate (pHRR), total heat release (THR), peak smoke production rate (pSPR), total smoke production (TSP), peak CO production rate (pCOPR), and peak CO2 production rate (pCO2PR) of EP/Mn3CoOx are reduced by 47.5 %, 21.5 %, 34.6 %, 17.6 %, 58.6 %, and 55.4 %, respectively. It has been shown that Mn3CoOx not only catalyzes the formation of high-quality char layer but also effectively catalyzes the conversion of hazardous gas products into CO2. Recovery experiments of Mn3CoOx filler in EP composites show that the recovery of Mn3CoOx can reach 90.0 %. This work provides insights into the design of efficient metal oxide flame retardants and ideas for the development of recycled flame retardants.

Analysis the Effect of Particle Size on the Ambient Temperature Oxidation Characteristics of Anthracite

ABSTRACT In order to study the oxidation characteristics of anthracite at ambient temperature. Anthracite coal samples of three particle sizes were chosen for oxidation in a closed space at 25°C, thus the characteristics of O2 consumption and CO production during ambient temperature oxidation of anthracite were obtained for different particle sizes. The results showed that the O2 consumption rate and CO production rate of anthracite during the ambient temperature oxidation process were large at the beginning and then gradually decrease and finally reach equilibrium. The O2 consumption rate increases with increasing particle size in the range of 0.05–1.00 mm. In contrast, the rate of CO production exhibited a nonlinear pattern, which was highest for the medium-sized coal samples and lower for the largest and smallest samples. The ambient temperature oxidation experiment was repeated on the oxidized coal samples after rinsing with fresh air, during which CO can still be produced and the time needed for the reaction to reach equilibrium was shortened. In addition, the consumption of O2 and the production of CO were much lower than those of the first oxidation, and the influence of particle size on both the rates of oxygen consumption and CO production exhibited a nonlinear correlation. Comparing the results of the two experiments, the oxidation rate was fastest for coal samples with a particle size of 0.10–0.50 mm, while the oxidation rate of coal decreased when the particle size of coal samples was less than 0.10 mm. The research has some reference significance for fire prevention in anthracite coal mines.

A highly stable TiO2/covalent organic framework heterojunction photocatalyst boosting charge transfer for visible-light-driven CO2 reduction

In this study, we present a novel heterojunction photocatalyst (TiO2-TTCOF) boosting charge transfer for visible-light-driven CO2 to CO conversion without photosensitizer or sacrificial agents. The 10% TiO2-TTCOF heterojunction photocatalyst is able to catalyze CO2 conversion, resulting in a highest CO production rate of 139.1 μmol g−1 with a selectivity of 96% and O2 production rate of 73.1 μmol g−1. Additionally, time-resolved fluorescence decay spectra confirmed the heterostructure between TTCOF and TiO2 can promote photoelectron transfer. The ATR-IFTS spectra indicated the photocatalytic reaction pathway.

Photothermal-driven CO2 reduction over Nd2O3/TiO2 heterojunction catalysts in aqueous medium

Elevated carbon dioxide levels, a major environmental concern, pose challenges for causing many climate problems. Addressing this, conversion CO2 into valuable chemicals is highly important. In this work, we explore photothermal catalytic CO2 reduction, an attractive approach that combines photocatalysis and thermal catalysis. We developed an enhanced Nd2O3/TiO2 catalyst using the sol-gel method, which significantly improves the efficiency of converting CO2 to CO in the presence of water. This catalyst exhibited a CO production rate of 22 μmol·gcat−1·h−1 at 130 °C, markedly surpassing the performance of sole photocatalysis by 7.3 times. Through systematic characterizations, we discovered that Nd2O3 prevents TiO2’s transition from anatase to rutile, thereby increasing CO2 adsorption and creating more vacancies. The interface between Nd2O3 and TiO2 forms a Z-scheme heterojunction, crucial for the simultaneous reduction of CO2 and oxidation of water. This research introduces a promising catalyst for photothermal CO2 reduction, which also acts as a reducing reagent. The strategic engineering of dual metal oxide interfaces in this catalyst suggests its applicability in a range of photothermal catalytic processes, marking a significant advancement in the field of CO2 utilization.

Bi2O2S/CAU-17 bifunctional heterojunction for boosting CO2 photoreduction performance origin from the simultaneous photoxidation of tetracycline

To address the issues of energy scarcity and environmental pollution, a photocatalytic coupling system is employed to simultaneously harness electrons and holes in a single photocatalytic system. The current study presents a novel approach to construct a dual reaction pathway system for tetracycline hydrochloride (TC) oxidation and CO2 reduction. Herein, Bi2O2S/CAU-17 composite was designed and fabricated through a facile solvothermal method. The hybrid photocatalyst exhibited an excellent performance for simultaneous TC degradation and CO2 reduction. The CO-production rate can be reached 22.0 μmol g-1h−1 through the optimized 20% Bi2O2S/CAU-17 sample. Notably, the source of CO2 in the reaction system is solely derived from the photoxidation of TC. The theoretical calculations and experimental findings have shown that the existed Bi2O2S can enrich electron and separation of photo-generated electrons from CAU-17, thus, the holes in Bi2O2S and CAU-17 can be involved in the photodegradation of TC. Afterwards, the CO2 generated by TC oxidation moves to Bi2O2S via diffusion of molecules and could be efficiently reduced by electrons to produce CO. The development of this novel bifunctional Bi2O2S/CAU-17 hybrid photocatalytic system could provide valuable insights for the advancement of photocatalytic coupling reaction systems.

Asymmetrical Interactions between Ni Single Atomic Sites and Ni Clusters in a 3D Porous Organic Framework for Enhanced CO2 Photoreduction.

3D porous organic frameworks, which possess the advantages of high surface area and abundant exposed active sites, are considered ideal platforms to accommodate single atoms (SAs) and metal nanoclusters (NCs) in high-performance catalysts; however, very little research has been conducted in this field. In the present work, a 3D porous organic framework containing Ni1 SAs and Nin NCs is prepared through the metal-assisted one-pot polycondensation of tetraaldehyde and hexaaminotriptycene. The single metal sites and metal clusters confined in the 3D space created a favorable micro-environment that facilitated the activation of chemically inert CO2 molecules, thus promoting the overall photoconversion efficiency and selectivity of CO2 reduction. The 3D-NiSAs/NiNCs-POPs, as a CO2 photoreduction catalyst, demonstrated an exceptional CO production rate of 6.24mmolg-1h-1, high selectivity of 98%, and excellent stability. The theoretical calculations uncovered that asymmetrical interaction between Ni1 SAs and Nin NCs not only favored the bending of CO2 molecules and reducing the CO2 reduction energy, but also regulated the electronic structure of the catalyst leading to the optimal binding strength of intermediates.

Construction of a hybrid flame retardant based on mesoporous silica for enhancing fire safety, smoke suppression, and mechanical properties of epoxy resins

AbstractIn order to improve the fire safety of epoxy resins (EPs), the SBA‐15 based hybrid flame retardant (SNAZD) was synthesized via an organic–inorganic hybridization strategy of mesoporous silica SBA‐15. Relying on electrostatic interaction, the zinc amino‐tris‐(methylenephosphonate) (Zn‐ATMP) was successfully introduced into the pore channels of SBA‐15. Then, 9,10‐dihydro‐9‐oxa‐10‐phosphaphenanthrene‐10‐oxide (DOPO) was successfully loaded into the pores of SBA‐15 under vacuum. The results show that the EP composites with the 5%SNAZD sample (sample EP‐5%SNAZD) showed a LOI value of 30.9% and achieved the vertical burning V‐0 rating. In comparison to EP, the peak heat release rate, peak smoke production rate, and production rate of CO of EP‐3%SNAZD were reduced by 32.2%, 31.9%, and 20.0%, respectively. This is due to the presence of Si, P, N, and Zn elements in the SNAZD, which promoted the generation of a high yield of dense char residue and inhibited the release of toxic gasses. And the impact strength and flexural strength of EP‐1%SNAZD were increased by 19.5% and 15.6%, respectively, and the E' of EP‐5%SNAZD increased by 49.1% when compared with the neat EP. This work provides a general strategy for the design of mesoporous hybrid flame retardant and creates additional opportunities for applications of EP.

A Comparative Study of Respiratory Activity of Tropical Products under Two Storage Conditions

This study aimed to investigate respiration process of Indonesian tropical products and its parameter to support the use of CAS. Shallot, dragon fruit and sneak fruit that are high-value and export-potential products in Indonesia were investigated. For respiration measurement, the fruits were kept in tightly closed jars. The ratio of fruit volume and free volume of jar (headspace) was determined to calculate the rate of fruit respiration. To observe the storage condition effects, the jars were stored in two different temperatures: low temperature (7±2°C) and room temperature (27±2°C). In cold temperature storage, changes in O2 and CO2 concentrations are slower than in room temperature storage. The rate of O2 consumption and CO2 production of products during storage decreased as the O2 concentration decreased for all conditions. Based on the dramatic increase of RQ value at low O2 concentrations, the low oxygen limits (LOLs) of shallot, sneak fruit and dragon fruit were estimated at around 7.5%, 4% and 2% O2 respectively, at the room temperature. However, the LOL was not detected yet at a cold temperature for 200 h of measurement due to a slow decrease of O2. The results showed that different products had different respiration activities so that the storage procedures should be different. A determination of model-based LOL and validation would be needed in the next research to be precisely applied on CAS. Keywords: Carbon dioxide, Dragon fruit, Shallot, Oxygen, Postharvest, Snake fruit.

Comprehensive evaluation of low-temperature oxidation characteristics of low-rank bituminous coal and oil shale

The coexistence of coal and oil shale mining conditions exacerbates the complexity of coal spontaneous combustion (CSC) prevention, so conducting in-depth research on the spontaneous combustion characteristics of coal, oil shale, and their mixed samples is necessary. A programmed heating system simulated the low-temperature oxidation process of bituminous coal and oil shale under different air volumes. It was found that CO concentration, C2H4 concentration, and Graham's fire coefficient (R1, R2) can be used as indicator gases to predict the CSC process. Compared with oil shale and mixed samples, bituminous coal has a higher CO production rate, oxygen consumption rate, heat release intensity, and lower apparent activation energy during the slow oxidation stage. Meanwhile, bituminous coal also has lower peak values of minimum float coal thickness, lower limit oxygen concentration, and maximal air leakage intensity, which means that bituminous coal in the goaf is more prone to oxidation. However, the abundant free hydrogen bonds in oil shale can stabilize the hydrogen-deficient functional groups of bituminous coal, which weakens the oxidation ability of the mixed sample during the accelerated oxidation stage. In addition, the increased air volume fraction increases the oxygen adsorption efficiency of the mixed sample throughout the low-temperature oxidation process, which means that the M70 sample has a higher CSC risk. The results have enriched the research on the spontaneous combustion characteristics of coal, oil shale, and mixed samples, which may strengthen the management and control of CSC in coal and oil shale co-mining mines.

The Pivotal Roles of Light and Ca‐Doping in Photothermocatalytic CO2 Reduction by Methane on Nanocomposites of Nickel Nanoparticles Loaded on Ca‐Doped Al2O3

CO2 and CH4 are greenhouse gases that can be converted into H2 and CO through light‐driven photothermocatalytic CO2 reduction with methane (CRM), which is a process of solar energy collection and storage. However, conventional catalysts require high light intensities (≥192.0 kW m−2) to obtain high fuel reaction rates and solar‐to‐fuel efficiency (η), and deactivate easily to coking at high temperature. Herein, a nanomaterial of Ni nanoparticles loaded on Ca‐doped Al2O3 (Ni/Ca–Al2O3) is synthesized. Ca doping improves the CO2 adsorption capacity of Ni/Ca–Al2O3. Under focused ultraviolet–visible–infrared illumination at low light intensity (80.8 kW m−2), Ni/Ca–Al2O3 obtains high production rates of H2 (, 76.85 mmol min−1 g−1) and CO (rCO, 90.90 mmol min−1 g−1), which are 1.9 and 1.3 times of those in the dark respectively, and exhibits a large η (30.3%) and good stability. The coking rate of Ni/Ca–Al2O3 is reduced by a factor of 25.8 compared to the reference catalyst with Ni nanoparticles loaded on Al2O3. The improvement of catalytic activity and anticoking properties stems from the photoactivation, which not only accelerates the CRM on Ni nanoparticles, but also enhances the oxidation of carbon species (produced on Ni nanoparticles) through strong adsorption of CO2 on Ca–Al2O3 at Ni/Ca–Al2O3 interface.

Co-pyrolysis model for polylactic acid (PLA)/wood composite and its application in predicting combustion behaviors

Polylactic acid (PLA)/wood composite has gained great popularity in applications due to its renewable and biodegradable features, whereas quantitative modelling from microscale co-pyrolysis to bench-scale combustion was barely reported. To challenge this issue, poplar wood, PLA and three PLA/wood composites with mass ratios of 1:3, 1:1, and 3:1 were adopted to conduct thermogravimetric analysis (TGA) and cone calorimeter tests. A numerical model was utilized to examine the interaction between wood and PLA during co-pyrolysis. Kinetics and temperature-dependent thermodynamics of each component were determined by inversely modelling some specific experimental results, while the remaining data were used for model validation. Effective heats of combustion of gas products were estimated by fitting the recorded heat release rates (HRR) in combustion tests. The results showed that PLA/wood composites considerably reduced the peak temperature of co-pyrolysis by 21.7–23.7 K compared to neat PLA. Pyrolysis of wood and PLA could be described by a four-component reaction scheme and a single-step reaction, respectively, whereas two additional reactions were needed to quantify the interaction between PLA and wood. Three methods were used to predict the measured HRRs, and all calculated curves fitted the experimental results well. PLA/wood composites decelerated the thickness regression rate and prolonged the combustion time. Meanwhile, measured CO and CO2 production rates were thoroughly analyzed.

Laminar burning velocity of lithium-ion battery thermal runaway vent gas in air

In this study, a spherically propagating flame of vent gas generated during the thermal runaway of lithium-ion batteries with different states of charge (SOC) was experimentally and numerically investigated. The vent gas is mainly composed of H2, CO, CO2, and some hydrocarbons. With increasing SOC, the CO2 fraction tends to decrease while the H2 and CO fractions tend to increase. Combustion experiments were conducted using a closed vessel, and the combustion progression was captured using a high-speed Schlieren image system to measure the unstretched laminar burning velocity, Su0. In addition, the combustion was computationally estimated under the experimental conditions by performing 1D planar flame simulations using Chemkin-Pro with the Aramco Mech 1.3 reaction model. Remarkably, the calculated values of Su0 closely matched the experimental ones, demonstrating good agreement. The results showed that Su0 tended to increase with increasing SOC. Furthermore, the effects of the chemical reaction mechanism, which plays a pivotal role in driving this increase in Su0 with increasing SOC, were investigated. Specifically, the heightened SOC levels promoted the H2 branching reaction led to an increased concentration of OH radicals in the mixture. This consequently accelerated the rate-determining reaction for the oxidation of hydrocarbons, leading to an increase in Su0. As an effect of the hydrocarbons in the vent gas mixtures, the number of moles of CO increased slightly near the flame because the rate of CO production in the flame zone was more dominant than that of consumption under the condition of SOC 50.

Polyarene Oxides with Tunable Quinone Units for Photocatalytic CO2 Reduction: A Simple Strategy toward Effective and Selective Catalysts.

The photocatalytic transformation of carbon dioxide (CO2) into valuable chemicals is a challenging process that requires effective and selective catalysts. However, most polymer-based photocatalysts with electron donor-acceptor (D-A) structures are synthesized with a fixed D-A ratio by using expensive monomers. Herein, we report a simple strategy to prepare polyarene oxides (PAOs) with quinone structural units via oxidation treatment of polyarene (PA). The resultant PAOs show tunable D-A structures and electronic band positions depending on the degree of oxidation, which can catalyze the photoreduction of CO2 with water under visible light irradiation, generating CO as the sole carbonaceous product without H2 generation. Especially, the PAO with an oxygen content of 17.6% afforded the highest CO production rate of 161.9 μmol g-1 h-1. It is verified that the redox transformation between quinone and phenolic hydroxyl in PAOs achieves CO2 photoreduction coupled with water oxidation. This study provides a facile way to access conjugated polymers with a tunable D-A structure and demonstrates that the resultant PAOs are promising photocatalysts for CO2 reduction.

Multiflower-like ReS2/NiAl-LDH Heterojunction for Visible-Light-Driven Photocatalytic CO2 Reduction.

The development of high-efficiency heterojunction photocatalysts has been recognized as an effective approach to facilitate photocatalytic CO2 reduction. In this research, we successfully synthesized a novel multiflower-like ReS2/NiAl-LDH heterojunction through a hydrothermal method. Remarkably, when exposed to visible-light irradiation, 2-ReS2/NiAl-LDH demonstrated an exceptional CO production rate of 272.26 μmol·g-1·h-1, which was 4.0 and 10.8 times higher than that of pristine NiAl-LDH and ReS2. The intertwined structure of ReS2 and NiAl-LDH promoted the efficient transfer and separation of photogenerated carriers, thereby significantly enhancing the photocatalytic CO2 reduction capabilities of the ReS2/NiAl-LDH. Furthermore, the carrier transfer pathway for the 2-ReS2/NiAl-LDH heterojunction was elucidated, suggesting a type II scheme mechanism, as evidenced by photochemical deposition experiments. The findings of this study offer valuable insights and pave the way for future research in the design and construction of LDH-based and ReS2-based heterojunctions for efficient photocatalytic CO2 reduction.

Variable frequency microwave induced CO2 Boudouard reaction over biochar

The Boudouard reaction presents promising application prospects as a straightforward and efficient method for CO2 conversion. However, its advancement is hindered primarily by elevated activation energy and a diminished conversion rate. This study employed a microwave reactor with a variable frequency as the initial approach to catalyze the CO2 Boudouard reaction over biochar, with the primary objective of producing renewable CO. The study systematically investigated the influence of various variables, including the heating source, microwave frequency, microwave power, gas hourly space velocity (GHSV), and carrier gas, on the conversion of CO2 and the selectivity towards CO. The experimental findings indicate that under static conditions, with a fixed microwave frequency set at 2450 MHz and 100 W microwave power, the Boudouard reaction did not initiate. Conversely, a CO2 conversion rate of 8.8% was achieved when utilizing a microwave frequency of 4225 MHz. Under this unique frequency, further elevating the microwave power to 275 W leads to the complete conversion of CO2. Furthermore, a comparative analysis between microwave and electrical heating revealed that the CO production rate was 37.7 μmol kJ−1 for microwave heating, in stark contrast to the considerably lower rate of 0.2 μmol kJ−1 observed for electric heating. Following the reaction, the biochar retained its robust 3D skeleton structure and abundant pore configuration. Notably, the dielectric constant increased by a factor of 1.8 compared to its initial state, rendering it a promising microwave-absorbing material.Graphical

High-efficiency photocatalytic CO2 reduction enabled by interfacial Ov and isolated Ti3+ of g-C3N4/TiO2 Z-scheme heterojunction

Exploring the real force that drives the separation of Coulomb-bound electron-hole pairs in the interface of heterojunction photocatalysts can establish a clear mechanism for efficient solar energy conversion efficiency. Herein, the formation of oxygen vacancy (Ov) and isolated Ti3+ was precisely regulated at the interface of g-C3N4/TiO2 Z-scheme heterojunction (g-C3N4/Ov-Ti3+-TiO2) by optimizing the opening degree of the calcination system, showing excellent production rate of CO and CH4 from CO2 photoreduction under visible light. This photocatalytic system also exhibited prominent stability. Combining theoretical calculation and characterization, the introduction of Ov and isolated Ti3+ on the interface could construct a charge transfer channel to break the forbidden transition of n → π*, improving the separation process of photoexcited electron-hole pairs. The photoexcited electrons weakened the covalent interaction of CO bonds to promote the activation of adsorbed inert CO2 molecules, significantly reducing the energy barrier of the rate-limiting step during CO2 reduction. This work demonstrates the great application potential of reasonably regulating heterojunction interface for efficient photocatalytic CO2 reduction.

Nanoflower-like TiO2/CoAl-layered double hydroxide direct Z-scheme for boosted photocatalytic CO2 conversion

Direct Z-scheme heterojunction (DZH) has promising potential in photocatalytic carbon dioxide reduction (PCR) owing to its unusual charge transfer pathway, exceptional charge separation efficiency, and high redox ability. Herein, ultrathin TiO2 nanosheets (NSs) have been employed as a substrate for the in-situ growth of CoAl layered double hydroxide (LDH) NSs to fabricate nanoflower-like TiO2/CoAl-LDH (TCA) DZH. The unconsolidated heterostructure is beneficial for active site exposure and mass transfer, and the inherent alkalinity of CoAl-LDH promoted the adsorption of CO2, synergistically boosting the process of PCR reaction in the TCA system. Simulated calculation and in-situ analysis jointly demonstrate the unique electron transfer processes during hybridization and photoexcitation. The resulting (-)TiO2/(+)CoAl-LDH interfacial electric field and DZH further lead to efficient separation of photogenerated charges of TCA. In the solid–gas system, the optimized TCA heterojunction exhibits a competitive PCR activity (76.18 μmol g−1h−1 for CO production rate) increase of 31.6 and 20.3 times compared to TiO2 and CoAl-LDH, respectively.

Assembling an S-type heterojunction comprising vacancy-rich CeO2-x and CuBi2O4 for improved photocatalytic oxidation of gaseous toluene

The exploration of highly efficient methods for degrading VOCs, with concurrent low energy consumption and lasting reusability, holds significant appeal. In this regard, an S-type CuBi2O4/CeO2-x heterojunction with the robust interfacial interactions is presented as an active photocatalyst for the efficient decomposition of gaseous toluene under full-spectrum irradiation. The optimal sample CC15 effectively degrades gaseous toluene at a high concentration of 1800 ppm within 2 h, achieving a notable CO2 yield of 87.05 %, and a TOC (total organic carbon) removal rate of 89.33 %. Furthermore, CuBi2O4/CeO2-x exhibits exceptional stability, maintaining its 100 % degradation capability over 32 cycles for nearly 64 h. Comparative characterization reveals that the superior performance derives from an abundance of oxygen vacancies and effective pre-adsorption capabilities, which facilitate rapid adsorption of VOCs on the catalyst surface, thereby increasing the likelihood of degradation reactions. Additionally, the formation of an S-type heterojunction, valence pairing between Bi3+ and Ce3+/4+ ions, and strong interfacial interactions serve as the primary pathways for the efficient separation of photogenerated carriers, contributing to the high CO2 production rate and prolonged cycle stability. The present investigation underscores the significant potential of vacancy-rich S-type heterojunctions and interfacial interactions between composite components, offering excellent activity and long-term availability for VOCs removal.

Study on experiments and numerical simulation of coal combustion characteristics under different thermal environments

In order to study heat release rate and flue gas generation during residual coal in goaf combustion, a cone calorimeter was used to research on combustion characteristics of bituminous coal under different heat radiation flux conditions. A novel coal fire FOAM solver for coal combustion is developed, numerically simulated by varying the gas atmosphere, and compared with the above experimental results. The results showed that with the increase in heat radiation flux, the shorter the time to reach the peak heat release rate, the greater the maximum heat release rate. When the coal does not enter the ignition stage, the CO production rate is higher than that after ignition, and the CO2 production rate is lower than that after ignition. Compared with the experimental results of the cone calorimeter, the difference between the two results is very small, which verified the feasibility and accuracy of the coal combustion model. After the injection of the composite inert gas, the heat release rate and mass loss rate of coal combustion have varying degrees of lag. The numerical simulation results can provide a theoretical basis for injecting inert compounds into the goaves of coal mines to prevent the spontaneous combustion of coal.

Ligand Mediated Assembly of CdS Colloids in 3D Porous Metal–Organic Framework Derived Scaffold with Multi‐Sites Heterojunctions for Efficient CO2 Photoreduction

AbstractThe inclusion of colloidal particles into 3D porous constructs to realize heterostructure ensembles enhances surface interactions and energy transfer that can transform the catalytic properties of conventional catalysts. However, assembling hydrophobic colloidal nanoparticles within hydrophilic 3D porous matrices to create tailored heterostructures and catalytic properties is particularly challenging. Here, a modified ligand grafting method is presented to spontaneously assemble CdS inorganic colloidal quantum dots within a metal‐organic framework (MOF) derived porous framework for efficient photocatalytic CO2 reduction. The grafted long chain molecular ligands effectively suppress phase separation and endow a molecular‐recognition effect to form ordered assembly microstructures. The proof‐of‐concept assembly of CdS and Prussian blue analogues (PBA) derived Co3O4 facilitates a high density of heterojunctions formation, improving charge transfer and extended lifetimes of photo‐induced electrons. Consequently, CdS/Co3O4 assembly exhibits exceptionally active and stable photocatalytic CO2 reduction activity, with a CO production rate of 73.9 µmol g−1 h−1 and CO selectivity of 98.9%. Importantly, the ligand grafting method can be generalized to achieve spontaneous assembly of quantum dots within various metal organic framework derived porous scaffolds. This work provides a rational strategy for precise self‐assembly of colloidal nanoparticles within porous microstructures, allowing tailored heterointerfaces for functional materials and applications.