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Polydimethylsilanediol synthesis method

A technology of polydimethylsilanediol and synthesis method, which is applied in the direction of silicon organic compounds, chemical instruments and methods, organic compounds/hydrides/coordination complex catalysts, etc., can solve environmental pollution and other problems, and achieve the difficulty of processing The effect of large size, elimination of pollution sources, and high treatment cost

Inactive Publication Date: 2014-08-27
杭州加农润滑材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This production method will produce a large amount of salty and VOC waste water during the alkaline cleaning process, which needs to be discharged, causing environmental pollution

Method used

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Experimental program
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Embodiment 1

[0022] (1) Raw materials: Hexamethylcyclotrisiloxane (D3) content ≥ 99.50%, about 140 kg;

[0023] 114 liters of deionized water is about 114 kg;

[0024] Industrially pure methanol, 21 liters, about 18 kg;

[0025] Cosolvent is selected 36 liters of acetone, about 28 kilograms;

[0026] Imidazolium salt analytical purity Purity ≥ 99% 15g;

[0027] Activated carbon industrial grade 100g;

[0028] Loaded salen catalyst 500g, self-made: condense (R,R)1,2-diphenylethylenediamine (DPEDA) 70g with 2-hydroxy-5-methyl-3-tert-butylbenzaldehyde 10g, temperature 110 ℃, to obtain chiral Salen, and then with Co(OAc)·4H 2 O35g is complexed and oxidized to obtain the Salen Co(III) chiral catalyst. Dissolve the salen catalyst in 500ML of ethanol and 500g of alumina, mix well and remove the ethanol to obtain the finished catalyst supported product. Catalyst synthesis route is as follows:

[0029]

[0030] (2) Production equipment

[0031] 1 set of 500L microwave and ultrasonic combine...

Embodiment 2

[0038] Concrete method is the same as embodiment 1, and difference is:

[0039] The first step is the synthesis reaction. 120kg of hexamethylcyclotrisiloxane, 105kg of deionized water, 18kg of methanol and 24kg of acetone are put into the microwave ultrasonic combined reactor system, and 500g of supported chiral catalyst (salen catalyst) is added, and the phase transfer Catalyst imidazolium salt 15g;

[0040] Second step is fractional distillation chromatography, adds 28kg water to the material that the first step reaction is completed;

[0041] In the third step, 100 g of activated carbon (0.67‰) was added to the obtained crude polydimethylsilanediol. Finally obtain about 129 kilograms of polydimethylsilanediol product.

Embodiment 3

[0043] Concrete method is the same as embodiment 1, and difference is:

[0044] The first step is the synthesis reaction. 145kg of hexamethylcyclotrisiloxane, 120kg of deionized water, 24kg of methanol and 36kg of acetone are put into the microwave ultrasonic combined reactor system, and 500g of supported chiral catalyst (salen catalyst) is added, and the phase transfer Catalyst imidazolium salt 15g;

[0045] Second step is fractional distillation chromatography, adds 30kg water to the material that the first step reaction is completed;

[0046] In the third step, 100 g of activated carbon (0.67‰) was added to the obtained crude polydimethylsilanediol. Finally obtain about 156 kilograms of polydimethylsilanediol product.

[0047] The yield of the polydimethylsilanediol product produced by the method of the present invention can reach more than 98%, and the product viscosity (25°C): 30-40mm 2 / s; ring body content: 15-20%; hydroxyl value: 9.0-11.5%, appearance: colorless and...

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Abstract

The present invention belongs to the field of organic chemistry, and particularly relates to a polydimethylsilanediol synthesis method. The method comprises the following steps: mixing hexamethyl cyclotrisiloxane, water, alcohol and cosolvent, then adding a supported chiral catalyst and a phase transfer catalyst, intensively mixing all the materials to form a miscible homogeneous phase and conducting reactions sufficiently to obtain the products of polydimethylsilanediol. The usage amount of hexamethyl cyclotrisiloxane, water and alcohol is determined according to the required polymerization degree of the products, and the specific ratio of hexamethyl cyclotrisiloxane, water and alcohol can be selected and adjusted according to the reaction formula. The method is green and environmental friendly, has zero discharge of wastewater and subsidiary reaction waste liquid, and truly achieves green and clean production in the premise of ensuring product quality.

Description

technical field [0001] The invention belongs to the field of organic chemistry, in particular to a method for synthesizing polydimethylsilanediol. Background technique [0002] Polydimethylsilanediol is a linear polysiloxane terminated by silanol groups, with a degree of polymerization of 6-9. Mainly used as: anti-structural control agent for methyl vinyl silicone rubber; finishing agent for cotton, silk, chemical fiber and other fabrics; peeling agent for artificial leather, etc. At present, the main process at home and abroad adopts the acetic anhydride method, that is, an acid-catalyzed ring-opening polymerization reaction is performed with methylcyclosiloxane and acetic anhydride, and then hydrolyzed and then neutralized by sodium bicarbonate or sodium carbonate for reflux alkaline washing reaction. During the alkaline cleaning process of this production method, a large amount of salty and VOC waste water will be produced, which needs to be discharged and cause environm...

Claims

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Application Information

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IPC IPC(8): C07F7/08B01J31/26
Inventor 翁华峰胡利华
Owner 杭州加农润滑材料有限公司
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