CN116139914A - Mor-containing molecular sieve composition for continuous synthesis of tertiary amine catalyst for polyurethane and preparation method thereof - Google Patents
Mor-containing molecular sieve composition for continuous synthesis of tertiary amine catalyst for polyurethane and preparation method thereof Download PDFInfo
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- CN116139914A CN116139914A CN202211388603.4A CN202211388603A CN116139914A CN 116139914 A CN116139914 A CN 116139914A CN 202211388603 A CN202211388603 A CN 202211388603A CN 116139914 A CN116139914 A CN 116139914A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
- B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
- B01J29/18—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the mordenite type
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D295/00—Heterocyclic compounds containing polymethylene-imine rings with at least five ring members, 3-azabicyclo [3.2.2] nonane, piperazine, morpholine or thiomorpholine rings, having only hydrogen atoms directly attached to the ring carbon atoms
- C07D295/02—Heterocyclic compounds containing polymethylene-imine rings with at least five ring members, 3-azabicyclo [3.2.2] nonane, piperazine, morpholine or thiomorpholine rings, having only hydrogen atoms directly attached to the ring carbon atoms containing only hydrogen and carbon atoms in addition to the ring hetero elements
- C07D295/023—Preparation; Separation; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D295/00—Heterocyclic compounds containing polymethylene-imine rings with at least five ring members, 3-azabicyclo [3.2.2] nonane, piperazine, morpholine or thiomorpholine rings, having only hydrogen atoms directly attached to the ring carbon atoms
- C07D295/02—Heterocyclic compounds containing polymethylene-imine rings with at least five ring members, 3-azabicyclo [3.2.2] nonane, piperazine, morpholine or thiomorpholine rings, having only hydrogen atoms directly attached to the ring carbon atoms containing only hydrogen and carbon atoms in addition to the ring hetero elements
- C07D295/027—Heterocyclic compounds containing polymethylene-imine rings with at least five ring members, 3-azabicyclo [3.2.2] nonane, piperazine, morpholine or thiomorpholine rings, having only hydrogen atoms directly attached to the ring carbon atoms containing only hydrogen and carbon atoms in addition to the ring hetero elements containing only one hetero ring
- C07D295/03—Heterocyclic compounds containing polymethylene-imine rings with at least five ring members, 3-azabicyclo [3.2.2] nonane, piperazine, morpholine or thiomorpholine rings, having only hydrogen atoms directly attached to the ring carbon atoms containing only hydrogen and carbon atoms in addition to the ring hetero elements containing only one hetero ring with the ring nitrogen atoms directly attached to acyclic carbon atoms
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2229/00—Aspects of molecular sieve catalysts not covered by B01J29/00
- B01J2229/30—After treatment, characterised by the means used
- B01J2229/32—Reaction with silicon compounds, e.g. TEOS, siliconfluoride
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2229/00—Aspects of molecular sieve catalysts not covered by B01J29/00
- B01J2229/30—After treatment, characterised by the means used
- B01J2229/37—Acid treatment
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Abstract
The invention relates to the technical field of molecular sieve catalysts, in particular to a mor-containing molecular sieve composition for continuously synthesizing tertiary amine catalysts for polyurethane and a preparation method thereof. The composition comprises the following raw materials in parts by weight: 30-35 parts of mor molecular sieve, 20-30 parts of alumina binder, 15-20 parts of extrusion aid and 2-4 parts of adhesive. The mor molecular sieve-containing composition prepared by the invention has the advantages that the mor molecular sieve is acidified, and then the novel molecular sieve catalyst obtained by silane hybridization is used, so that the use of morpholine can be reduced, and the utilization rate of morpholine can be improved. The mor-containing molecular sieve composition prepared by the invention reduces the consumption of expensive raw material morpholine, thereby reducing the production cost of synthesizing N-methylmorpholine for enterprises.
Description
Technical Field
The invention relates to the technical field of molecular sieve catalysts, in particular to a mor-containing molecular sieve composition for continuously synthesizing tertiary amine catalysts for polyurethane and a preparation method thereof.
Background
N-methylmorpholine is an important intermediate in organic chemical industry, and is a colorless to yellow liquid compound with amine taste, and the chemical formula is C5H11NO. CAS number 109-02-4, molecular weight 101.15, has dual properties of tertiary amine and ether, and is widely used as chemical intermediate, extractant, corrosion inhibitor, surfactant, etc., in polyurethane industry, N-methylmorpholine is used as catalyst for polyester polyurethane soft foam.
The synthesis process of N-methylmorpholine is many, and according to the raw material, there are morpholine method, N-methyldiethanol method, diethanolamine method, diglycol method and dichloroethyl ether method, wherein methylation research using morpholine as raw material is the most studied, and is also an important method for synthesizing N-methylmorpholine. The morpholine methylation method has high price of raw material morpholine, needs noble metal catalyst, has high production cost, and simultaneously generates a large amount of industrial wastewater containing formaldehyde, which is difficult to treat. Other methods basically adopt concentrated sulfuric acid for dehydration, and have high three wastes and low yield.
Based on the above circumstances, the invention provides a mor-containing molecular sieve composition for continuous synthesis of tertiary amine catalysts for polyurethane and a preparation method thereof.
Disclosure of Invention
The invention aims to provide a mor-containing molecular sieve composition for continuous synthesis of a tertiary amine catalyst for polyurethane and a preparation method thereof.
In order to achieve the above object, the present invention provides a mor molecular sieve-containing composition for continuous synthesis of tertiary amine catalyst for polyurethane, the composition comprising the following raw materials in parts by weight: 30-35 parts of mor molecular sieve, 20-30 parts of alumina binder, 15-20 parts of extrusion aid and 2-4 parts of adhesive.
Preferably, the alumina binder is one of aluminum nitrate, aluminum sulfate, aluminum chloride, aluminum hydroxide, sodium metaaluminate, pseudo-boehmite, and aluminum isopropoxide.
Preferably, the extrusion aid is selected from one or more than two of starch, sesbania powder, hydroxyethyl methylcellulose, methylcellulose and polyethylene glycol.
Preferably, the binder is a 3% nitric acid solution by mass.
Preferably, the mor molecular sieve is treated by the following method steps:
(1) Uniformly mixing a mor molecular sieve and an organic weak acid solution according to the mass ratio of 1g (mor molecular sieve) of 20-25 ml (organic weak acid solution), stirring for 2-2.5 h at the temperature of 30-35 ℃, filtering, washing with deionized water, and drying at the temperature of 60-70 ℃ to constant weight to obtain the mor molecular sieve modified by the organic weak acid;
(2) Mixing organic weak acid modified mor molecular sieve and toluene in the mass ratio of 1g (mor molecular sieve) to 50-60 ml (toluene) to form toluene suspension, adding organosilane in the mass ratio of 1g (mor molecular sieve) to 30-40 ml (organosilane) into toluene suspension, mixing uniformly, stirring at 25-30 deg.C for 24 hr, filtering, washing filter residue with absolute ethyl alcohol for 3 times, centrifuging, vacuum drying for 12 hr to obtain the invented product.
Preferably, the weak organic acid in the step (1) is one of acetic acid, oxalic acid, benzoic acid, sorbic acid, citric acid and malic acid.
Preferably, the concentration of the weak organic acid solution in the step (2) is 7.0-8.0 mol/L.
Preferably, the organosilane is an organosilane containing a trimethoxy structure.
Preferably, the organosilane containing trimethoxy structure has the general formula C X H Y O Z Si, wherein X is more than or equal to 5 and Z is less than or equal to 5.
Preferably, the organic silane containing a trimethoxy structure is one of phenyl trimethoxy silane, 3-glycidol ether oxygen propyl trimethoxy silane, 3-aminopropyl trimethoxy silane, 3-chloropropyl trimethoxy silane and vinyl trimethoxy silane.
Preferably, the organosilane containing a trimethoxy structure is phenyl trimethoxysilane.
The invention also provides a preparation method of the mor molecular sieve-containing composition for continuously synthesizing the tertiary amine catalyst for polyurethane, which comprises the following steps:
(1) Uniformly mixing a mor molecular sieve and an organic weak acid solution according to the mass ratio of 1g (mor molecular sieve) of 20-25 ml (organic weak acid solution), stirring for 2-2.5 h at the temperature of 30-35 ℃, filtering, washing with deionized water, and drying at the temperature of 60-70 ℃ to constant weight to obtain the mor molecular sieve modified by the organic weak acid;
(2) Mixing organic weak acid modified mor molecular sieve and toluene in the mass ratio of 1g (mor molecular sieve) to 50-60 ml (toluene) to form toluene suspension, adding organosilane in the mass ratio of 1g (mor molecular sieve) to 30-40 ml (organosilane) into toluene suspension, mixing uniformly, stirring at 25-30 ℃ for 24h, filtering, washing filter residue with absolute ethyl alcohol for 3 times, centrifuging, vacuum drying for 12h to obtain silane hybridized mor molecular sieve;
(3) Kneading the silane hybridized mor molecular sieve with an alumina binder, an extrusion aid and an adhesive, fully rolling, extruding strips, drying at 100+/-5 ℃ for 10-12 h, roasting at 550-600 ℃ for 4.5-5.0 h, and crushing into particles with 20-30 meshes to obtain the silica gel.
The invention also provides application of the mor-containing molecular sieve composition in the process of synthesizing tertiary amine catalysts for polyurethane.
The tertiary amine catalyst process for synthesizing polyurethane is a process of generating N-methylmorpholine by reacting morpholine with methanol.
Compared with the prior art, the invention has the following beneficial effects:
1. the mor molecular sieve-containing composition prepared by the invention has the advantages that the mor molecular sieve is acidified, and then the novel molecular sieve catalyst obtained by silane hybridization is used, so that the use of morpholine can be reduced, and the utilization rate of morpholine can be improved. The mor-containing molecular sieve composition prepared by the invention reduces the consumption of expensive raw material morpholine, thereby reducing the production cost of synthesizing N-methylmorpholine for enterprises.
2. The raw materials of the invention are abundant in China and have proper price, so that the large-scale production of the invention has no high cost limit; meanwhile, the preparation method is simple, the overall production cost is low, and the method is beneficial to industrial mass production.
Detailed Description
Example 1
The specific raw materials are weighed according to table 1, and the preparation steps are as follows:
(1) Mixing the mor molecular sieve and the acetic acid solution uniformly, stirring for 2.5 hours at the temperature of 30 ℃, filtering, washing with deionized water, and drying to constant weight at the temperature of 60 ℃ to obtain the mor molecular sieve modified by organic weak acid;
(2) Mixing organic weak acid modified mor molecular sieve and toluene uniformly to form toluene suspension, adding organosilane into the toluene suspension, mixing uniformly, stirring for 24 hours at 25 ℃, filtering, washing filter residues with absolute ethyl alcohol for 3 times, centrifuging, and drying in vacuum for 12 hours to obtain silane hybridized mor molecular sieve;
(3) Mixing and kneading the silane hybridized mor molecular sieve with pseudo-boehmite, sesbania powder and nitric acid solution (3%), fully rolling, extruding strips, drying at 100+/-5 ℃ for 10 hours, roasting at 550 ℃ for 5.0 hours, and crushing into particles with 20-30 meshes to obtain the silica gel.
Example 2
The specific raw materials are weighed according to table 1, and the preparation steps are as follows:
(1) Mixing the mor molecular sieve and the acetic acid solution uniformly, stirring for 2 hours at the temperature of 35 ℃, filtering, washing with deionized water, and drying at the temperature of 70 ℃ to constant weight to obtain the mor molecular sieve modified by organic weak acid;
(2) Mixing organic weak acid modified mor molecular sieve and toluene uniformly to form toluene suspension, adding organosilane into the toluene suspension, mixing uniformly, stirring for 24 hours at 30 ℃, filtering, washing filter residues with absolute ethyl alcohol for 3 times, centrifuging, and drying in vacuum for 12 hours to obtain silane hybridized mor molecular sieve;
(3) Mixing and kneading the silane hybridized mor molecular sieve with pseudo-boehmite, sesbania powder and nitric acid solution (3%), fully rolling, extruding strips, drying at 100+/-5 ℃ for 12 hours, roasting at 600 ℃ for 4.5 hours, and crushing into particles with 20-30 meshes to obtain the silica gel.
Example 3
The specific raw materials are weighed according to table 1, and the preparation steps are as follows:
(1) Mixing the mor molecular sieve and the acetic acid solution uniformly, stirring for 2.5 hours at the temperature of 35 ℃, filtering, washing with deionized water, and drying to constant weight at the temperature of 70 ℃ to obtain the mor molecular sieve modified by organic weak acid;
(2) Mixing organic weak acid modified mor molecular sieve and toluene uniformly to form toluene suspension, adding organosilane into the toluene suspension, mixing uniformly, stirring for 24 hours at 30 ℃, filtering, washing filter residues with absolute ethyl alcohol for 3 times, centrifuging, and drying in vacuum for 12 hours to obtain silane hybridized mor molecular sieve;
(3) Mixing and kneading the silane hybridized mor molecular sieve with pseudo-boehmite, sesbania powder and nitric acid solution (3%), fully rolling, extruding strips, drying at 100+/-5 ℃ for 12 hours, roasting at 600 ℃ for 5.0 hours, and crushing into particles with 20-30 meshes to obtain the silica gel.
Comparative example 1
Specific raw materials were weighed according to table 1, except that the mor molecular sieve was not subjected to silane hybridization treatment, and the remaining steps were prepared as follows:
(1) Mixing the mor molecular sieve and the acetic acid solution uniformly, stirring for 2.5 hours at the temperature of 35 ℃, filtering, washing with deionized water, and drying to constant weight at the temperature of 70 ℃ to obtain the mor molecular sieve modified by organic weak acid;
(2) Mixing and kneading the mor molecular sieve modified by organic weak acid with pseudo-boehmite, sesbania powder and nitric acid solution (3%), extruding strips after full rolling, drying for 12 hours at 100+/-5 ℃, roasting for 5.0 hours at 600 ℃, and crushing into particles with 20-30 meshes to obtain the modified mor molecular sieve.
Comparative example 2
Specific raw materials were weighed according to table 1, and the preparation procedure was as follows, except that the organosilane was vinyltrimethoxysilane, as in example 3:
(1) Mixing the mor molecular sieve and the acetic acid solution uniformly, stirring for 2.5 hours at the temperature of 35 ℃, filtering, washing with deionized water, and drying to constant weight at the temperature of 70 ℃ to obtain the mor molecular sieve modified by organic weak acid;
(2) Mixing organic weak acid modified mor molecular sieve and toluene uniformly to form toluene suspension, adding organosilane into the toluene suspension, mixing uniformly, stirring for 24 hours at 30 ℃, filtering, washing filter residues with absolute ethyl alcohol for 3 times, centrifuging, and drying in vacuum for 12 hours to obtain silane hybridized mor molecular sieve;
(3) Mixing and kneading the silane hybridized mor molecular sieve with pseudo-boehmite, sesbania powder and nitric acid solution (3%), fully rolling, extruding strips, drying at 100+/-5 ℃ for 12 hours, roasting at 600 ℃ for 5.0 hours, and crushing into particles with 20-30 meshes to obtain the silica gel.
Comparative example 3
Specific raw materials were weighed according to table 1, and unlike example 3, the organosilane was 3-aminopropyl trimethoxysilane, and the remaining steps were prepared as follows:
(1) Mixing the mor molecular sieve and the acetic acid solution uniformly, stirring for 2.5 hours at the temperature of 35 ℃, filtering, washing with deionized water, and drying to constant weight at the temperature of 70 ℃ to obtain the mor molecular sieve modified by organic weak acid;
(2) Mixing organic weak acid modified mor molecular sieve and toluene uniformly to form toluene suspension, adding organosilane into the toluene suspension, mixing uniformly, stirring for 24 hours at 30 ℃, filtering, washing filter residues with absolute ethyl alcohol for 3 times, centrifuging, and drying in vacuum for 12 hours to obtain silane hybridized mor molecular sieve;
(3) Mixing and kneading the silane hybridized mor molecular sieve with pseudo-boehmite, sesbania powder and nitric acid solution (3%), fully rolling, extruding strips, drying at 100+/-5 ℃ for 12 hours, roasting at 600 ℃ for 5.0 hours, and crushing into particles with 20-30 meshes to obtain the silica gel.
Comparative example 4
Specific raw materials were weighed according to table 1, and unlike example 3, the organosilane was 3-glycidoxypropyl trimethoxysilane, the remaining steps were prepared as follows:
(1) Mixing the mor molecular sieve and the acetic acid solution uniformly, stirring for 2.5 hours at the temperature of 35 ℃, filtering, washing with deionized water, and drying to constant weight at the temperature of 70 ℃ to obtain the mor molecular sieve modified by organic weak acid;
(2) Mixing organic weak acid modified mor molecular sieve and toluene uniformly to form toluene suspension, adding organosilane into the toluene suspension, mixing uniformly, stirring for 24 hours at 30 ℃, filtering, washing filter residues with absolute ethyl alcohol for 3 times, centrifuging, and drying in vacuum for 12 hours to obtain silane hybridized mor molecular sieve;
(3) Mixing and kneading the silane hybridized mor molecular sieve with pseudo-boehmite, sesbania powder and nitric acid solution (3%), fully rolling, extruding strips, drying at 100+/-5 ℃ for 12 hours, roasting at 600 ℃ for 5.0 hours, and crushing into particles with 20-30 meshes to obtain the silica gel.
TABLE 1
EXAMPLE 4 evaluation of the catalytic Synthesis of N-methylmorpholine from morpholine and methanol
With 10m each of examples 1 to 3 and comparative examples 1 to 4 prepared 3 Reactor to be charged into an industrial plant with 0.2m 3 Metal catalyst (Cr 5%, cu22%, tiO) 2 1%, pt0.5%, the balance being Ni), the molar ratio of morpholine to methanol input per hour is 1:15, preheating, vaporizing and mixing with circulating hydrogen gas, entering a reactor, controlling the reaction pressure to be 0.6Mpa, controlling the reaction temperature to be 150 ℃ and the reaction time to be 3 hours, cooling the reacted crude N-methylmorpholine by heat exchange, entering a crude N-methylmorpholine storage tank, and sampling and analyzing by gas chromatography. The conversion efficiency results are shown in Table 2.
Taking 10m each of example 3 and comparative examples 3, 4 3 Reactor to be charged into an industrial plant with 0.2m 3 Metal catalyst (Cr 5%, cu22%, tiO) 2 1%, pt0.5%, the balance being Ni) per hourThe mole ratio of input morpholine to methanol is 1:25, preheating, vaporizing and mixing with circulating hydrogen gas, feeding into a reactor, controlling the reaction pressure to be 0.6Mpa, controlling the reaction temperature to be 150 ℃ and the reaction time to be 3 hours, feeding the reacted crude N-methylmorpholine into a crude N-methylmorpholine storage tank after heat exchange cooling, and sampling and analyzing by gas chromatography. The conversion efficiency results are shown in Table 3.
Taking 10m each of example 3 and comparative example 4 3 Reactor to be charged into an industrial plant with 0.2m 3 Metal catalyst (Cr 5%, cu22%, tiO) 2 1%, pt0.5%, the balance being Ni), the molar ratio of morpholine to methanol input per hour is 1:30, preheating, vaporizing and mixing with circulating hydrogen, entering a reactor, controlling the reaction pressure to be 0.6Mpa, controlling the reaction temperature to be 150 ℃ and the reaction time to be 3 hours, cooling the reacted crude N-methylmorpholine by heat exchange, entering a crude N-methylmorpholine storage tank, and sampling and analyzing by gas chromatography. The conversion efficiency results are shown in Table 4.
TABLE 2
TABLE 3 Table 3
TABLE 4 Table 4
The foregoing descriptions of specific exemplary embodiments of the present invention are presented for purposes of illustration and description. It is not intended to limit the invention to the precise form disclosed, and obviously many modifications and variations are possible in light of the above teaching. The exemplary embodiments were chosen and described in order to explain the specific principles of the invention and its practical application to thereby enable one skilled in the art to make and utilize the invention in various exemplary embodiments and with various modifications as are suited to the particular use contemplated. It is intended that the scope of the invention be defined by the claims and their equivalents.
Claims (10)
1. A mor-containing molecular sieve composition for continuous synthesis of tertiary amine catalysts for polyurethane, which is characterized by comprising the following raw materials in parts by weight: 30-35 parts of mor molecular sieve, 20-30 parts of alumina binder, 15-20 parts of extrusion aid and 2-4 parts of adhesive.
2. The mor-containing molecular sieve composition of claim 1, wherein the SAPO-34 molecular sieve is treated by the following method steps:
(1) Uniformly mixing a mor molecular sieve and an organic weak acid solution according to the mass ratio of 1g (mor molecular sieve) of 20-25 ml (organic weak acid solution), stirring for 2-2.5 h at the temperature of 30-35 ℃, filtering, washing with deionized water, and drying at the temperature of 60-70 ℃ to constant weight to obtain the mor molecular sieve modified by the organic weak acid;
(2) Mixing organic weak acid modified mor molecular sieve and toluene in the mass ratio of 1g (mor molecular sieve) to 50-60 ml (toluene) to form toluene suspension, adding organosilane in the mass ratio of 1g (mor molecular sieve) to 30-40 ml (organosilane) into toluene suspension, mixing uniformly, stirring at 25-30 deg.C for 24 hr, filtering, washing filter residue with absolute ethyl alcohol for 3 times, centrifuging, vacuum drying for 12 hr to obtain the invented product.
3. The mor-containing molecular sieve composition of claim 2, wherein the weak organic acid in step (1) is one of acetic acid, oxalic acid, benzoic acid, sorbic acid, citric acid, and malic acid.
4. The mor-containing molecular sieve composition of claim 2, wherein the concentration of the weak organic acid solution in step (2) is from 7.0 to 8.0mol/L.
5. The mor-containing molecular sieve composition of claim 2, wherein the organosilane is an organosilane containing a trimethoxy structure.
6. The mor-containing molecular sieve composition of claim 5, wherein the organosilane having a trimethoxy structure has the formula C X H Y O Z Si, wherein X is more than or equal to 5 and Z is less than or equal to 5.
7. The mor-containing molecular sieve composition of claim 6, wherein the organosilane containing a trimethoxy structure is one of phenyl trimethoxysilane, 3-glycidoxypropyl trimethoxysilane, 3-aminopropyl trimethoxysilane, 3-chloropropyl trimethoxysilane, vinyl trimethoxysilane.
8. The mor-containing molecular sieve composition of claim 7, wherein the organosilane containing a trimethoxy structure is phenyl trimethoxysilane.
9. The mor-containing molecular sieve composition of claim 2, wherein the mor-containing molecular sieve composition is prepared by a process comprising:
(1) Uniformly mixing a mor molecular sieve and an organic weak acid solution according to the mass ratio of 1g (mor molecular sieve) of 20-25 ml (organic weak acid solution), stirring for 2-2.5 h at the temperature of 30-35 ℃, filtering, washing with deionized water, and drying at the temperature of 60-70 ℃ to constant weight to obtain the mor molecular sieve modified by the organic weak acid;
(2) Mixing organic weak acid modified mor molecular sieve and toluene in the mass ratio of 1g (mor molecular sieve) to 50-60 ml (toluene) to form toluene suspension, adding organosilane in the mass ratio of 1g (mor molecular sieve) to 30-40 ml (organosilane) into toluene suspension, mixing uniformly, stirring at 25-30 ℃ for 24h, filtering, washing filter residue with absolute ethyl alcohol for 3 times, centrifuging, vacuum drying for 12h to obtain silane hybridized mor molecular sieve;
(3) Kneading the silane hybridized mor molecular sieve with an alumina binder, an extrusion aid and an adhesive, fully rolling, extruding strips, drying at 100+/-5 ℃ for 10-12 h, roasting at 550-600 ℃ for 4.5-5.0 h, and crushing into particles with 20-30 meshes to obtain the silica gel.
10. Use of the mor-containing molecular sieve composition according to any one of claims 1 to 9 in a tertiary amine-based catalyst process for the synthesis of polyurethane, wherein the tertiary amine-based catalyst process for the synthesis of polyurethane is a process in which morpholine is reacted with methanol to form N-methylmorpholine.
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