CN110124536B - Organic-inorganic dual-functional-layer reverse osmosis membrane - Google Patents
Organic-inorganic dual-functional-layer reverse osmosis membrane Download PDFInfo
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- CN110124536B CN110124536B CN201910483857.6A CN201910483857A CN110124536B CN 110124536 B CN110124536 B CN 110124536B CN 201910483857 A CN201910483857 A CN 201910483857A CN 110124536 B CN110124536 B CN 110124536B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0079—Manufacture of membranes comprising organic and inorganic components
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/12—Composite membranes; Ultra-thin membranes
- B01D69/125—In situ manufacturing by polymerisation, polycondensation, cross-linking or chemical reaction
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/56—Polyamides, e.g. polyester-amides
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/441—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by reverse osmosis
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/36—Hydrophilic membranes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/124—Water desalination
- Y02A20/131—Reverse-osmosis
Abstract
The invention provides an organic-inorganic dual-function layer reverse osmosis membrane which comprises a supporting layer, a polyamide function layer and a molecular sieve function layer which are sequentially connected, wherein the polyamide function layer is formed by interfacial polymerization of a polyamine-containing aqueous phase solution and a molecular sieve particle-containing organic phase solution, and the molecular sieve particle and a molecular sieve of the molecular sieve function layer belong to the same topological structure. According to the invention, the hydrophilic molecular sieve is loaded on the surface of the polyamide reverse osmosis membrane in a hydrothermal synthesis manner, so that the binding force between the molecular sieve and the polyamide membrane layer is improved, the hydrophilic modification capacity of the polyamide reverse osmosis membrane is obviously improved, and the polyamide reverse osmosis membrane has wide application prospects in various fields of municipal or industrial sewage treatment, seawater desalination, brackish water desalination, fruit juice concentration and the like.
Description
Technical Field
The invention belongs to the technical field of membrane separation, and particularly relates to a reverse osmosis membrane which can be applied to the fields of municipal or industrial sewage treatment, seawater desalination and the like.
Background
The reverse osmosis technology is a widely used separation technology, and is widely used in various fields such as municipal or industrial sewage treatment, seawater desalination, brackish water desalination, fruit juice concentration and the like. In the field of reverse osmosis membranes, the most common reverse osmosis membrane is a polyamide reverse osmosis membrane, which is relatively low in price and good in thermochemical stability and can meet most reverse osmosis requirements. But their permeability, including salt rejection and water flux, generally limits their application in certain fields.
In order to modify the permeability, inorganic nanoparticles with hydrophilic function are often used to modify polyamide to improve its hydrophilicity. Molecular sieve is a common polyamide modified additive, and has been widely noticed by scholars because of its regular pore structure. For inorganic modified polyamide mills, three common modification modes are support layer doping, interfacial polymerization doping and membrane surface coating, and compared with other modification modes, the membrane surface coating has more improved hydrophilicity compared with other modes due to the hydrophilic coating straight fabric liquid layer. However, for the molecular sieve coating, the molecular sieve coating is rarely used for modifying the polyamide membrane, because the molecular sieve coating is gradually reduced due to physical reasons such as liquid scouring and the like in the application process, and the performance of the membrane is reduced, so that the application of the polyamide membrane is limited.
Disclosure of Invention
In order to solve the problems, the invention provides a reverse osmosis membrane, which loads a hydrophilic molecular sieve on the surface of a polyamide reverse osmosis membrane in a hydro-thermal synthesis mode, so that the binding force between the molecular sieve and a polyamide membrane layer is improved, and the hydrophilic modification capacity of the polyamide reverse osmosis membrane is obviously improved.
The invention provides an organic-inorganic dual-function layer reverse osmosis membrane which comprises a supporting layer, a polyamide function layer and a molecular sieve function layer which are sequentially connected, wherein the polyamide function layer is formed by interfacial polymerization of a polyamine-containing aqueous phase solution and a molecular sieve particle-containing organic phase solution, and the molecular sieve particle and a molecular sieve of the molecular sieve function layer belong to the same topological structure.
The molecular sieve functional layer is a continuous and compact molecular sieve layer and has a reverse osmosis desalination function.
The molecular sieve functional layer is a discontinuous molecular sieve layer and does not have a reverse osmosis desalination function.
The molecular sieve functional layer is formed by taking molecular sieve particles in the polyamide functional layer as nucleation centers and performing hydrothermal crystallization.
The molecular sieve is NaA molecular sieve.
The invention also provides a preparation method of the organic-inorganic dual-functional layer reverse osmosis membrane, which comprises the following steps:
(1) dissolving 0.5-5wt% of polyamine in water to form an aqueous phase solution, and dispersing 0.5-5wt% of polybasic acyl chloride and 0.2-2wt% of molecular sieve particles in an organic solvent to form an organic phase solution;
(2) immersing the support layer into the aqueous phase solution, taking out the support layer for 5-30s, removing the aqueous phase solution on the surface of the support layer, immersing the support layer into the organic phase solution, taking out the support layer after 5-30s, removing the organic phase solution on the surface, and placing the support layer in an oven at 50-100 ℃ for thermal crosslinking to form a polyamide membrane;
(3) immersing the support layer side of the polyamide membrane into an alcohol solution dispersed with phenolic resin for 1-3min, and continuously drying in a drying oven at 50-100 ℃;
(4) immersing the polyamide membrane treated in the step (3) into a molecular sieve synthetic liquid containing a silicon source, an aluminum source, an alkali source and water for hydrothermal crystallization so as to form a molecular sieve functional layer;
(5) and (4) completely immersing the membrane crystallized in the step (4) into an alcohol solution for treatment for 5-10min, and cleaning, soaking and drying the membrane by pure water to form the organic-inorganic dual-function layer reverse osmosis membrane.
The polyamine is selected from one or more of m-phenylenediamine, piperazine, p-phenylenediamine, ethylenediamine, propylenediamine, hexamethylenediamine, o-phenylenediamine, melamine and diaminotoluene, and the polybasic acyl chloride is selected from one or more of trimesoyl chloride, phthaloyl chloride, isophthaloyl chloride, terephthaloyl chloride, phthaloyl chloride, butanetriacyl chloride, pentanedioyl chloride, hexanetrioyl chloride, cyclopropanetriacyl chloride, cyclobutanetriacyl chloride, cyclobutane tetracoyl chloride, cyclopentane triacyl chloride, cyclopentane tetracoyl chloride, cyclohexane triacyl chloride and cyclohexane tetracoyl chloride.
When a molecular sieve functional layer with a reverse osmosis function needs to be formed, Na in the molecular sieve synthetic liquid2O、Al2O3、SiO2And H2The molar ratio of O is (2-3) to (1-7) to (150-300), the crystallization temperature is 50-80 ℃, and the crystallization time is 4-6 h.
When a molecular sieve functional layer without reverse osmosis function needs to be formed, Na in the molecular sieve synthetic liquid2O、Al2O3、SiO2And H2The molar ratio of O is (2-3) to (1-3) to (100-180), the crystallization temperature is 90-100 ℃, and the crystallization time is 1-2 h.
The aluminum source is sodium aluminate, aluminum powder, sodium metaaluminate or aluminum hydroxide; the silicon source is sodium silicate, silica sol or sodium metasilicate.
The alcohol in the step (3) and the step (5) is one of methanol, ethanol, isopropanol and propanol.
The invention has the beneficial effects that: according to the invention, the formation of the molecular sieve functional layer is promoted by taking the physically doped molecular sieve in the polyamide functional layer as a nucleation center, so that the binding force between the molecular sieve and the polyamide is remarkably improved, and the possibility that the molecular sieve is physically washed away in the application process is avoided. And secondly, the hydrophilic capacity of the support layer, the polyamide functional layer and the molecular sieve functional layer is increased progressively, so that the hydrophilic capacity of the polyamide membrane is maximized. In addition, aiming at different requirements of different fields on high desalination rate and high water flux of the reverse osmosis membrane, the invention can also prepare membrane materials with different properties by adjusting the synthesis conditions of the molecular sieve functional layer, and has wide application range.
Detailed Description
The invention is further illustrated with reference to specific examples.
Example 1
The embodiment relates to an organic-inorganic dual-function layer reverse osmosis membrane which comprises a supporting layer, a polyamide function layer and a molecular sieve function layer which are sequentially connected, wherein the polyamide function layer is formed by interfacial polymerization of a water phase solution containing polyamine and an organic phase solution containing molecular sieve particles and polybasic acyl chloride, the molecular sieves of the molecular sieve particles and the molecular sieve function layer are both NaA molecular sieves, and the molecular sieve function layer is a continuous and compact molecular sieve layer and has a reverse osmosis desalination function.
The reverse osmosis membrane is prepared by the following method:
(1) dissolving 2wt% of piperazine in water to form an aqueous phase solution, and dispersing 0.5 wt% of trimesoyl chloride and 1 wt% of NaA molecular sieve particles in an organic solvent to form an organic phase solution;
(2) immersing a polysulfone supporting layer into the aqueous phase solution, taking out the polysulfone supporting layer for 30s, removing the aqueous phase solution on the surface of the supporting layer, immersing the polysulfone supporting layer into the organic phase solution, taking out the polysulfone supporting layer after 30s, removing the organic phase solution on the surface, and placing the polysulfone supporting layer into a 60 ℃ oven for thermal crosslinking to form a polyamide membrane;
(3) immersing the support layer side of the polyamide membrane into an ethanol solution dispersed with phenolic resin for 3min, and continuously placing the polyamide membrane into a 60 ℃ drying oven for drying;
(4) immersing the polyamide membrane treated in the step (3) into a molecular sieve synthetic solution containing silica sol, sodium metaaluminate, sodium hydroxide and water for hydrothermal crystallization to form a molecular sieve functional layerIn the examples, Na is contained in the molecular sieve synthesis solution2O、Al2O3、SiO2And H2The molar ratio of O is 2:1:5:150, the crystallization temperature is 80 ℃, and the crystallization time is 6 hours.
(5) And (4) completely immersing the membrane crystallized in the step (4) into an ethanol solution for treatment for 10min, and cleaning, soaking and drying by pure water to form the organic-inorganic dual-function layer reverse osmosis membrane.
Example 2
The embodiment relates to an organic-inorganic dual-function layer reverse osmosis membrane which comprises a supporting layer, a polyamide function layer and a molecular sieve function layer which are sequentially connected, wherein the polyamide function layer is formed by interfacial polymerization of a water phase solution containing polyamine and an organic phase solution containing molecular sieve particles and polybasic acyl chloride, the molecular sieves of the molecular sieve particles and the molecular sieve function layer are both NaA molecular sieves, and the molecular sieve function layer is a discontinuous molecular sieve layer and does not have a reverse osmosis desalination function. The reverse osmosis membrane is prepared by the following method:
(1) dissolving 2wt% of piperazine in water to form an aqueous phase solution, and dispersing 0.5 wt% of trimesoyl chloride and 1 wt% of NaA molecular sieve particles in an organic solvent to form an organic phase solution;
(2) immersing a polysulfone supporting layer into the aqueous phase solution, taking out the polysulfone supporting layer for 30s, removing the aqueous phase solution on the surface of the supporting layer, immersing the polysulfone supporting layer into the organic phase solution, taking out the polysulfone supporting layer after 30s, removing the organic phase solution on the surface, and placing the polysulfone supporting layer into a 60 ℃ oven for thermal crosslinking to form a polyamide membrane;
(3) immersing the support layer side of the polyamide membrane into an ethanol solution dispersed with phenolic resin for 3min, and continuously placing the polyamide membrane into a 60 ℃ drying oven for drying;
(4) immersing the polyamide membrane treated in the step (3) into a molecular sieve synthetic solution containing silica sol, sodium metaaluminate, sodium hydroxide and water for hydrothermal crystallization to form a molecular sieve functional layer, in this example, Na in the molecular sieve synthetic solution2O、Al2O3、SiO2And H2The molar ratio of O is 2:1:3:160, the crystallization temperature is 90 ℃, and the crystallization time is 2 hours.
(5) And (4) completely immersing the membrane crystallized in the step (4) into an ethanol solution for treatment for 10min, and cleaning, soaking and drying by pure water to form the organic-inorganic dual-function layer reverse osmosis membrane.
Example 3
The embodiment relates to a single-functional-layer reverse osmosis membrane which comprises a supporting layer and a polyamide functional layer which are sequentially connected, wherein the polyamide functional layer is formed by interfacial polymerization of an aqueous phase solution containing polyamine and an organic phase solution containing molecular sieve particles and polybasic acyl chloride, and the molecular sieve particles are NaA molecular sieves.
The reverse osmosis membrane is prepared by the following method:
(1) dissolving 2wt% of piperazine in water to form an aqueous phase solution, and dispersing 0.5 wt% of trimesoyl chloride and 1 wt% of NaA molecular sieve particles in an organic solvent to form an organic phase solution;
(2) and (2) firstly immersing the polysulfone supporting layer into the aqueous phase solution, taking out the polysulfone supporting layer for 30s, removing the aqueous phase solution on the surface of the supporting layer, immersing the polysulfone supporting layer into the organic phase solution, taking out the polysulfone supporting layer after 30s, removing the organic phase solution on the surface, and placing the polysulfone supporting layer into a 60 ℃ oven for thermal crosslinking to form a polyamide layer so as to form the reverse osmosis membrane.
Example 4
The embodiment relates to a single-functional-layer reverse osmosis membrane which comprises a supporting layer, a polyamide functional layer and a molecular sieve functional layer which are sequentially connected, wherein the polyamide functional layer is formed by interfacial polymerization of a polyamine-containing aqueous phase solution and a molecular sieve particle and polyacyl chloride-containing organic phase solution, and the molecular sieve particle is a NaA molecular sieve.
The reverse osmosis membrane is prepared by the following method:
(1) dissolving 2wt% of piperazine in water to form an aqueous phase solution, and dispersing 0.5 wt% of trimesoyl chloride and 1 wt% of NaA molecular sieve particles in an organic solvent to form an organic phase solution;
(2) and (3) immersing the polysulfone supporting layer into the aqueous phase solution, taking out the polysulfone supporting layer for 30s, removing the aqueous phase solution on the surface of the supporting layer, immersing the polysulfone supporting layer into the organic phase solution, taking out the polysulfone supporting layer after 30s, removing the organic phase solution on the surface, and placing the polysulfone supporting layer into an oven at 60 ℃ for thermal crosslinking to form a polyamide layer.
(3) The surface of the polyamide membrane is soaked in a suspension containing 2wt% of NaA molecular sieve and 1 wt% of hydroxypropyl cellulose, the soaking time is 2min, and after the soaking is finished, the membrane is placed in a 60 ℃ oven to be dried, so that the organic-inorganic dual-function layer reverse osmosis membrane is formed.
Example 5
The embodiment relates to an organic-inorganic dual-function layer reverse osmosis membrane which comprises a supporting layer, a polyamide function layer and a molecular sieve function layer which are sequentially connected, wherein the polyamide function layer is formed by interfacial polymerization of a water phase solution containing polyamine and an organic phase solution containing molecular sieve particles and polybasic acyl chloride, the molecular sieves of the molecular sieve particles and the molecular sieve function layer are both NaA molecular sieves, and the molecular sieve function layer is a continuous and compact molecular sieve layer and has a reverse osmosis desalination function.
The reverse osmosis membrane is prepared by the following method:
(1) dissolving 2wt% of piperazine in water to form an aqueous phase solution, and dispersing 0.5 wt% of trimesoyl chloride and 1 wt% of NaA molecular sieve particles in an organic solvent to form an organic phase solution;
(2) immersing a polysulfone supporting layer into the aqueous phase solution, taking out the polysulfone supporting layer for 30s, removing the aqueous phase solution on the surface of the supporting layer, immersing the polysulfone supporting layer into the organic phase solution, taking out the polysulfone supporting layer after 30s, removing the organic phase solution on the surface, and placing the polysulfone supporting layer into a 60 ℃ oven for thermal crosslinking to form a polyamide membrane;
(3) immersing the polyamide membrane into a molecular sieve synthetic solution containing silica sol, sodium metaaluminate, sodium hydroxide and water for hydrothermal crystallization to form a molecular sieve functional layer, in this example, Na is contained in the molecular sieve synthetic solution2O、Al2O3、SiO2And H2The molar ratio of O is 2:1:5:150, the crystallization temperature is 80 ℃, and the crystallization time is 6 hours; and cleaning with pure water, soaking and drying to form the organic-inorganic dual-functional layer reverse osmosis membrane.
Example 6
The embodiment relates to an organic-inorganic dual-function layer reverse osmosis membrane which comprises a supporting layer, a polyamide function layer and a molecular sieve function layer which are sequentially connected, wherein the polyamide function layer is formed by interfacial polymerization of a water phase solution containing polyamine and an organic phase solution containing molecular sieve particles and polybasic acyl chloride, the molecular sieves of the molecular sieve particles and the molecular sieve function layer are both NaA molecular sieves, and the molecular sieve function layer is a discontinuous molecular sieve layer and does not have a reverse osmosis desalination function. The reverse osmosis membrane is prepared by the following method:
(1) dissolving 2wt% of piperazine in water to form an aqueous phase solution, and dispersing 0.5 wt% of trimesoyl chloride and 1 wt% of NaA molecular sieve particles in an organic solvent to form an organic phase solution;
(2) immersing a polysulfone supporting layer into the aqueous phase solution, taking out the polysulfone supporting layer for 30s, removing the aqueous phase solution on the surface of the supporting layer, immersing the polysulfone supporting layer into the organic phase solution, taking out the polysulfone supporting layer after 30s, removing the organic phase solution on the surface, and placing the polysulfone supporting layer into a 60 ℃ oven for thermal crosslinking to form a polyamide membrane;
(3) immersing the polyamide membrane into a molecular sieve synthetic solution containing silica sol, sodium metaaluminate, sodium hydroxide and water for hydrothermal crystallization to form a molecular sieve functional layer, in this example, Na is contained in the molecular sieve synthetic solution2O、Al2O3、SiO2And H2The molar ratio of O is 2:1:3:160, the crystallization temperature is 90 ℃, and the crystallization time is 2 hours; and cleaning with pure water, soaking and drying to form the organic-inorganic dual-functional layer reverse osmosis membrane.
The reverse osmosis membranes prepared in examples 1 to 6 were tested for NaCl salt rejection and water flux in 2000ppm NaCl aqueous solution under the test conditions of an operating pressure of 225psi, a temperature of 25 ℃, and a pH value of 7, and the test results of all the reverse osmosis membranes after 1h and 144h of operation are summarized in table 1 below.
TABLE Performance test results for Polyamide reverse osmosis membranes prepared in different examples
As can be seen from the above table, the bifunctional layer polyamide membrane prepared in example 1 has better salt rejection, and the bifunctional layer polyamide membrane prepared in example 2 has better water flux, and the permeation performance does not decrease with the increase of the test time, compared to the reverse osmosis polyamide membrane of example 3, which only contains a single polyamide functional layer. While example 4, which was coated with only the molecular sieve coating, had comparable initial performance to example 2, but its performance decreased significantly with longer test times. While examples 5 and 6 demonstrate the necessity of plugging the pores of the support layer prior to hydrothermal synthesis.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (4)
1. The preparation method of the organic-inorganic dual-functional-layer reverse osmosis membrane is characterized in that the reverse osmosis membrane comprises a supporting layer, a polyamide functional layer and a molecular sieve functional layer which are sequentially connected, wherein the polyamide functional layer is formed by interfacial polymerization of a water phase solution containing polyamine and an organic phase solution containing molecular sieve particles and polyacyl chloride, and the molecular sieve particles and the molecular sieve of the molecular sieve functional layer belong to the same topological structure; the molecular sieve functional layer is a continuous and compact molecular sieve layer and has a reverse osmosis desalination function; the preparation method comprises the following steps:
dissolving 0.5-5wt% of polyamine in water to form an aqueous phase solution, and dispersing 0.5-5wt% of polybasic acyl chloride and 0.2-2wt% of molecular sieve particles in an organic solvent to form an organic phase solution;
immersing the support layer into the aqueous phase solution, taking out the support layer for 5-30s, removing the aqueous phase solution on the surface of the support layer, immersing the support layer into the organic phase solution, taking out the support layer after 5-30s, removing the organic phase solution on the surface, and placing the support layer in an oven at 50-100 ℃ for thermal crosslinking to form a polyamide membrane;
immersing the support layer side of the polyamide membrane into an alcohol solution dispersed with phenolic resin for 1-3min, and continuously drying in a drying oven at 50-100 ℃;
immersing the polyamide membrane treated in the step (3) into a molecular sieve synthetic liquid containing a silicon source, an aluminum source, an alkali source and water for hydrothermal crystallization so as to form a molecular sieve functional layer;
completely immersing the membrane crystallized in the step (4) into an alcohol solution for treatment for 5-10min, and cleaning, soaking and drying with pure water to form an organic-inorganic dual-function layer reverse osmosis membrane; na in the molecular sieve synthetic solution2O、Al2O3、SiO2And H2The molar ratio of O is (2-3) to (1-7) to (150-300), the crystallization temperature is 50-80 ℃, and the crystallization time is 4-6 h.
2. The method of claim 1, wherein the molecular sieve is a NaA molecular sieve.
3. The method according to claim 1, wherein the polyamine is selected from one or more of m-phenylenediamine, piperazine, p-phenylenediamine, ethylenediamine, propylenediamine, hexamethylenediamine, o-phenylenediamine, melamine and diaminotoluene, and the poly-acid chloride is selected from one or more of poly-acid chloride compounds selected from trimesoyl chloride, phthaloyl chloride, isophthaloyl chloride, terephthaloyl chloride, phthaloyl chloride, butanetriacyl chloride, pentatriacyl chloride, hexanetrioyl chloride, cyclopropanetriacyl chloride, cyclobutanetriacyl chloride, cyclobutane tetracoyl chloride, cyclopentane triacyl chloride, cyclopentane tetracoyl chloride, cyclohexane triacyl chloride and cyclohexane tetracoyl chloride.
4. The process of claim 1, characterized in that the aluminum source is sodium aluminate, aluminum powder, sodium metaaluminate, or aluminum hydroxide; the silicon source is sodium silicate, silica sol or sodium metasilicate.
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