Method for synthesizing sulfonic acid resin catalyst used for polyoxymethylene dimethyl ethers efficiently

A technology of polyoxymethylene dimethyl ether and sulfonic acid resin, applied in chemical instruments and methods, organic compound/hydride/coordination complex catalyst, catalyst activation/preparation, etc., can solve the problem of lower yield and non-recyclable Problems such as use, liquid acid catalyst and product are difficult to separate

Inactive Publication Date: 2016-08-10
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, its disadvantage is that it corrodes the equipment, cannot be recycled, and the liquid acid catalyst and the product are evenly mixed and difficult to separate
[0010] 2. Solid super acid catalyzed method, Zhao Feng et al. (Zhao Feng, Li Huaju, Song Huanling, et al. Paraformaldehyde and methanol in SO 4 2 - / Fe 2 o 3 Research on Ring-opening Condensation Reaction on Solid Superacid[J]. Natural Gas Chemical Industry: C1 Chemistry and Chemical Industry, 2013,38 (1):1-6.) Selection of Solid Superacid SO 4 2- / Fe 2 o 3 As a catalyst, DMMn was synthesized from methanol and paraformaldehyde, and the reaction DMM 3-8 The yield is 22%, and the reason that yield is less is that a large amount of water is generated in the reaction process, and the synthetic DMMn hydrolysis reaction generates hemiacetal, reduces yield
But in the reaction process, how to adjust the acidity of the catalyst to make it more suitable for the production of DMMn with a chain length of n=3-4, and to increase the DMM 3-8 The yield still needs to be further studied

Method used

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  • Method for synthesizing sulfonic acid resin catalyst used for polyoxymethylene dimethyl ethers efficiently
  • Method for synthesizing sulfonic acid resin catalyst used for polyoxymethylene dimethyl ethers efficiently
  • Method for synthesizing sulfonic acid resin catalyst used for polyoxymethylene dimethyl ethers efficiently

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Put 3 grams of NKC-9 sulfonic acid tree catalyst into 100 mL containing insoluble alcohol solvent (methanol, ethanol, propanol, ethylene glycol, 1,3-propanediol, 2-propanol, n-butanol, n-pentanol , Isoamyl alcohol, n-hexanol, cyclohexanol, benzyl alcohol, etc.) in the reaction kettle, treat the sulfonic acid resin catalyst in the temperature range of 70-140 ℃ for 1-8h. The treated catalyst was filtered and dried in an oven at 120 °C for 6 h. The evaluation conditions of the catalyst were as follows: 60 mL of DMM, 20 g of paraformaldehyde, and 3 g of the modified sulfonic acid resin catalyst were weighed and added to the reaction kettle respectively. use N 2 Replace the air in the kettle three times under the condition of 1.0 MPa, so that the remaining air content in the kettle is lower than 0.1%. Into 2.0 MPa of N 2 , let it stand for 30 minutes, and use it for leak testing of the reactor to ensure that the device is airtight and then evacuate the gas in the reactor....

Embodiment 2

[0033] The polystyrene sulfonic acid resin catalyst (D-009B, DA-330, D-006, D-072, Amberlyst-15, NKC-9) of 3g different models is packed in the reactor containing benzyl alcohol solvent of 100mL, in 100-150 ℃, 5.0 MPa, under CO atmosphere for 1h. The treated catalyst was filtered and dried in an oven at 120 °C for 6 h. The catalyst evaluation conditions are as follows: Weigh 60 mL of DMM, 20 g of paraformaldehyde, and 3 g of modified sulfonic acid resin catalyst, and add them into the reaction kettle respectively. use N 2 Replace the air in the kettle three times under the condition of 1.0 MPa, so that the remaining air content in the kettle is lower than 0.1%. Into 2.0 MPa of N 2 , let it stand for 30 minutes, and use it for leak testing of the reactor to ensure that the device is airtight and then evacuate the gas in the reactor. Pass again 2.0 MPa N 2 , the stirring speed of the reactor was 500 rpm, the reaction temperature was controlled at 90 °C, and the reaction tim...

Embodiment 3

[0038] Put 3g of NKC-9 catalyst into a 100ml reaction kettle containing benzyl alcohol solvent, and treat it at 130°C, 5.0 MPa, and CO atmosphere for 0.5-20 h. After the treated catalyst was filtered, it was dried in an oven at 120 °C for 6 h. The evaluation conditions of the catalyst were as follows: 60 mL of DMM, 20 g of paraformaldehyde, and 3 g of the modified sulfonic acid resin catalyst were weighed and added to the reaction kettle respectively. use N 2 Replace the air in the kettle three times under the condition of 1.0 MPa, so that the remaining air content in the kettle is lower than 0.1%. N passing through 2.0 MPa 2 , let it stand for 30 minutes, and use it for leak testing of the reactor to ensure that the device is airtight and then evacuate the gas in the reactor. Pass again 2.0 MPaN 2 , the stirring speed of the reactor was 500 rpm, the reaction temperature was controlled at 90 °C, and the reaction time was 3 h.

[0039] Table 3. The effect of different cata...

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Abstract

The invention provides a method for synthesizing a sulfonic acid resin catalyst used for polyoxymethylene dimethyl ethers efficiently, and relates to a method for synthesizing a resin catalyst. The method comprises: a modified method for synthesizing sulfonic acid resin catalyst used for polyoxymethylene dimethyl ethers efficiently by using methylal and trioxymethylene as raw materials. The polar organic alcohol solvent is selected to heat the sulfonic acid resin catalyst for 0.5-20 hours in the presence of CO under 0.1-20.0 MPa at 50-200 DEG C, and the polar organic alcohol solvent used as a water-carrying agent and a pore-enlarging agent works together with a structural modifier of sulfonic acid resin. The method uses the polar organic alcohol solvent to heat the sulfonated polystyrene resin catalyst, and the polar organic alcohol solvent used as the water-carrying agent and the pore-enlarging agent works together with the structural modifier of sulfonic acid resin. The polar organic alcohol solvent shows good reaction activity between methylal and trioxymethylene and good selectivity of product DMM<3-8>.

Description

technical field [0001] The invention relates to a method for synthesizing a resin catalyst, in particular to a method for efficiently synthesizing a polyoxymethylene dimethyl ether sulfonic acid resin catalyst. Background technique [0002] Polyoxymethylene dimethyl ether (DMMn) is a general term for a class of substances, and its simplified formula can be expressed as: CH 3 O (CH 2 O) n CH 3 , wherein n is an integer ≥ 1, and the synthetic raw materials of DMMn mainly include two parts, one part is a compound that provides paraformaldehyde, including formaldehyde solution, paraformaldehyde, paraformaldehyde, etc.; the other part provides end-capping compounds, including methanol, Dimethyl ether, methylal, etc., see reaction equation (1, 2) for details. [0003] 2CH 3 OH+CH 2 O→CH 3 OCH 2 OCH 3 +H 2 O……………………………………………………….(1) [0004] 2CH 3 OH+nCH 2 O→CH 3 O (CH 2 O) n CH 3 +H 2 O………………………………………………(2) [0005] DMMn in which the length of n is between 3-8 i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/10C07C41/56C07C43/30
CPCB01J31/10B01J37/0009C07C41/56C07C43/30
Inventor 石磊孙东张婉莹陈飞张晓东
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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