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Preparation method of hydrogenation catalyst and method for preparing dimethylaminopropylamine diisopropanol

A technology of dimethylaminopropylamine diisopropanol and hydrogenation catalyst is applied in the preparation of organic compounds, molecular sieve catalysts, chemical instruments and methods, etc., and can solve relatively high safety requirements, unknown product purity, and low yield of main products. and other problems, to achieve the effects of good economy, improved activity and stability, and high product purity

Pending Publication Date: 2022-02-01
WANHUA CHEM GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Through preliminary calculation, the yield is about 86%, but the purity of the obtained product is unknown
[0012] Therefore at present the synthesis of dimethylaminopropylamine diisopropanol all adopts the batch process with N,N-dimethyl-1,3-propanediamine and propylene oxide, and this process adopts flammable and explosive propylene oxide, It has a certain degree of danger, and the safety requirements for industrial production are relatively high. In addition, there are problems such as high by-products, low yield of main products, and low product purity.

Method used

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  • Preparation method of hydrogenation catalyst and method for preparing dimethylaminopropylamine diisopropanol
  • Preparation method of hydrogenation catalyst and method for preparing dimethylaminopropylamine diisopropanol
  • Preparation method of hydrogenation catalyst and method for preparing dimethylaminopropylamine diisopropanol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0062] 1# Catalyst precursor preparation:

[0063] To 90g HZSM-5 (silicon-aluminum ratio is 200) and 10g ZrSi 2 Add 2g of citric acid, 2g of methyl cellulose and 1g of kale powder, mix evenly, add 10g of deionized water and knead evenly, extrude the block into a cylindrical shape with an extruder, and dry it at 110°C after natural air drying 6h, roasted at 450°C for 6h to get 90%HZSM-5+10%ZrSi 2 Composite carrier.

[0064] Use 100ml of deionized water to prepare an impregnating solution containing 20g of nickel, 2g of ruthenium, and 0.5g of zinc nitrate, and add 77.5g of the above-mentioned composite carrier by equal volume impregnation method. After 24h, the adsorption equilibrium is reached, and then dried at 110°C for 6h, and then dried at 500°C Calcined at the bottom for 8h to obtain 1# catalyst precursor, its mass composition is: 20%Ni+2%Ru+0.5%Zn / 90%HZSM-5+10%ZrSi 2 .

[0065] Synthesis of dimethylaminopropylamine diisopropanol:

[0066] In a stainless steel catalyt...

Embodiment 2

[0069] 2# Catalyst precursor preparation:

[0070] To 95g HZSM-5 (silicon-aluminum ratio is 100) and 5g ZrSi 2 Add 1g of nitric acid, 4g of polyvinyl alcohol and 5g of graphite to the mixture, mix well, add 10g of deionized water and knead evenly, extrude the block into a clover shape with an extruder, and dry it naturally at 100°C for 8h, then at 300°C Roast for 12 hours to get 95% HZSM-5+5% ZrSi 2 Composite carrier.

[0071] Use 100ml of deionized water to prepare an impregnation solution containing 15g of nickel, 0.3g of chromium, and 0.2g of iron nitrate, and add 84.5g of the above-mentioned composite carrier by the equal volume impregnation method. After 24h, the adsorption balance is reached, and then dried at 100°C for 8h, 400 Calcined at ℃ for 10h to obtain 2# catalyst precursor, its mass composition is: 15%Ni+0.3%Cr+0.2%Fe / 95%HZSM-5+5%ZrSi 2 .

[0072] Synthesis of dimethylaminopropylamine diisopropanol:

[0073] In a stainless steel catalytic rectification tower...

Embodiment 3

[0076] 3# Catalyst precursor preparation:

[0077] To 88g HZSM-5 (silicon-aluminum ratio is 400) and 12g ZrSi 2 Add 4g of boric acid, 1g of soluble starch and 3g of scallop powder, mix evenly, add 20g of deionized water and knead evenly, extrude the block into a cross core shape with an extruder, and dry it naturally at 80°C for 12h. Calcined at 500°C for 8h to get 88%HZSM-5+12%ZrSi 2 Composite carrier.

[0078] Use 100ml of deionized water to prepare an impregnation solution containing 10g of nickel, 2.0g of chromium, and 1.0g of zinc nitrate, and add 87.0g of the above-mentioned composite carrier by equal volume impregnation method. After 24h, the adsorption balance is reached, and then dried at 80°C for 12h, 600 Calcined at ℃ for 6h to obtain 3# catalyst precursor, its mass composition is: 10%Ni+2%Cr+1%Zn / 88%HZSM-5+12%ZrSi 2 .

[0079] Synthesis of dimethylaminopropylamine diisopropanol:

[0080]In a stainless steel catalytic rectification tower with an internal diamet...

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Abstract

The invention provides a preparation method of a hydrogenation catalyst and a method for preparing dimethylaminopropylamine diisopropanol by using the catalyst. A carrier of the catalyst is an HZSM-5 and ZrSi2 composite carrier, and active components of the catalyst are Ni and an auxiliary agent thereof. The catalyst can be used for preparing dimethylaminopropylamine diisopropanol by taking dimethylaminopropionitrile, diisopropanolamine and hydrogen as raw materials, has the advantages of high activity, high selectivity and stable performance, can run for a long period, and reduces the production cost. In addition, a new reaction route is adopted, epoxypropane is not used, the danger of the process can be reduced, the dimethylaminopropylamine diisopropanol is continuously produced by adopting a catalytic rectifying tower, the conditions are mild, the product yield is high (greater than 92%), few impurities are difficult to separate, the product purity is high (greater than 99.5%), the economical efficiency is good, and the method has a good application prospect.

Description

technical field [0001] The invention belongs to the field of catalyst preparation and application, and in particular relates to a method for preparing a hydrogenation catalyst and a method for preparing dimethylaminopropylamine diisopropanol. Background technique [0002] The polyurethane foaming system mainly includes polyisocyanates, polyols, catalysts, surfactants, etc. Among them, tertiary amine catalysts are mostly used as catalysts, which have certain catalytic effects on foaming reaction and gel reaction. At present, the bulk tertiary amine catalysts on the market, such as N, N-dimethylcyclohexylamine, pentamethyldiethylenetriamine, triethylenediamine, etc., are mostly small molecule products that are easy to emit, and there are nasty The amine odor will continue to migrate out during the construction process or from the foam product, causing harm to human health. As environmental protection requirements become higher and higher, low-VOC catalysts will become an inev...

Claims

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Application Information

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IPC IPC(8): B01J29/40B01J29/46B01J29/48C07C213/08C07C215/14
CPCB01J29/405B01J29/46B01J29/48C07C213/08B01J2229/18C07C215/14
Inventor 刘振国张聪颖孔令健周亚文沈雨晗王洪刚黄圣兵
Owner WANHUA CHEM GRP
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