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Continuous preparation method of electronic-grade methyl silicone oil

A technology of methyl silicone oil and electronic grade, which is applied in the field of continuous preparation of electronic grade methyl silicone oil, can solve the problems of design improvement and poor effect, and achieve the effect of stable polymerization and high conversion rate

Active Publication Date: 2020-12-29
HUBEI XINGRUI SILICON MATERIAL CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The metal ions come from the raw materials and the kettle body; the low boilers are mainly due to the design of the de-lowering process and equipment needs to be improved; the hydroxyl content in the methyl silicone oil mainly comes from the moisture in the raw materials, but the main raw material hexamethyldisilaz The boiling point of oxane is 99.5°C, which is close to that of water, and the traditional distillation principle is not effective. Therefore, it is necessary to study the continuous preparation method of electronic grade silicone oil.

Method used

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  • Continuous preparation method of electronic-grade methyl silicone oil

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] 10kg octamethylcyclotetrasiloxane (D 4 ) mixed with 2kg crown ether mixture A (100 parts of crown ether mixture A contains 35 parts of 12-crown 4-ether, 35 parts of 15-crown ether-5, 30 parts of 18-crown ether-6), and the temperature and pressure of the rectification tower is 20kpa Under the condition, the fraction D at 130℃ was collected 4 -21; Mix 1kg of hexamethyldisiloxane (MM) and 200g of crown ether mixture A evenly, and collect the fraction MM-11 at 70°C under the condition of temperature and pressure of the rectification tower at 20kpa, and M-11 is treated by two-stage 4A molecular sieve adsorption The device removes water, and stays in the primary and secondary 4A molecular sieve adsorption treatment devices for 24h and 24h respectively, and the pretreated product is recorded as MM-21 (water content is 8ppm); raw material D 4 -21 and MM-21 are input into the screw mixer at a mass flow rate of 100:1.5, and mixed at 65±3°C to obtain premix D 4 MM-21; Premix D a...

Embodiment 2

[0022] In addition to octamethylcyclotetrasiloxane (D 4 ) and crown ether mixture A are 10kg and 1kg respectively, hexamethyldisiloxane (MM) and crown ether mixture A (20 parts of 4-nitrobenzo-15-crown 5-ether, dibenzo-18 - 60 parts of -crown-6-ether, 20 parts of 1-aza-12-crown 4-ether) were 1 kg and 100 g respectively, the other processes and steps were the same as in Example 1 to obtain the finished product PDMS-312. The polymerization conversion rate is 89.1%, and the finished product PDMS-312 test index: viscosity 315mm 2 / s, molecular weight distribution coefficient 1.52, low boiler 0.11%, silanol content 6ppm, Na ion content 9ppb, K ion content 6ppb, Cu ion content 6ppb, Pb ion content 8ppb, As ion content 9ppb, Fe ion content 12ppb. ,

Embodiment 3

[0024] In addition to octamethylcyclotetrasiloxane (D 4 ) and crown ether mixture A are 10kg and 400g respectively, hexamethyldisiloxane (MM) and crown ether mixture A (35 parts of 24-crown 8-ether, 22 parts of benzo-12-crown ether-4, Except that 36 parts of 4-aminobenzo-15-crown-5-ether and 7 parts of aza-18-crown ether) were 1kg and 40g respectively, other processes and steps were the same as in Example 1 to obtain the finished product PDMS-313. The polymerization conversion rate is 89.0%, and the finished product PDMS-313 test index: viscosity 311mm 2 / s, molecular weight distribution coefficient 1.63, low boiler 0.11%, silanol content 6ppm, Na ion content 25ppb, K ion content 36ppb, Cu ion content 21ppb, Pb ion content 18ppb, As ion content 20ppb, Fe ion content 45ppb.

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Abstract

The invention relates to a continuous preparation method of electronic-grade methyl silicone oil, which comprises the following steps: pretreating raw materials: carrying out metal complexing agent rectification purification or molecular sieve adsorption treatment and metal complexing agent rectification purification on the raw materials and auxiliary materials in series for use; premixing the rawmaterials: inputting the pretreated raw materials into a screw mixer according to a certain mass ratio, and performing heat preservation and mixing; polymerization: inputting the premixed material into a first-stage static fluidized bed for prepolymerization, and then inputting into a second-stage static fluidized bed for equilibrium polymerization to obtain a semi-finished product; and carryingout low-boiling-point substance removal: inputting the semi-finished product into a film evaporator, primarily removing low-boiling-point substances through first-stage purification, and then inputting the semi-finished product into a short-path low-molecular distiller for second-stage purification to obtain a finished product. The process is a continuous production process, polymerization is stable, the conversion rate is high, the finished product indexes are as follows: the molecular weight distribution coefficient is small, the low-boiling-point substance content is less than 0.20%, the silicon hydroxyl content is low, the Na, K and heavy metal ion content is less than 10ppb, and the application requirements of industries such as electronics, microelectronics and the like can be met.

Description

technical field [0001] The invention relates to the technical field of preparation of methyl silicone oil, in particular to a continuous preparation method of electronic grade methyl silicone oil. Background technique [0002] Methyl silicone oil is a kind of organosilicon polymer with flexible chain polysiloxane as the main chain and silicon methyl end cap. According to the difference of polymer quality and specification, it can be used as lubricant, brightener, release agent, Defoamers, plasticizers and other additives are widely used in industries such as machinery, petroleum, electric power, plastics, rubber, coatings, textiles, food and fermentation, medical care and sanitation. At present, domestic commercially available methyl silicone oil is mainly characterized by high content of metal ions such as potassium, sodium and heavy metals, which is close to hundreds of ppm, high content of low boiling substances such as dimethylsiloxane ring body greater than 0.50%, and h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/06C08G77/04C08G77/08C08G77/34
CPCC08G77/06C08G77/04C08G77/08C08G77/34
Inventor 徐小刚孙刚杜斌陈泽雨龚俊英陈海平
Owner HUBEI XINGRUI SILICON MATERIAL CO LTD
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