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A kind of preparation method of mq resin with narrow molecular weight distribution

A narrow molecular weight distribution and resin technology, which is applied in the field of MQ resin preparation with narrow molecular weight distribution, can solve problems such as MQ resins that have not been discussed, and achieve the effects of high product quality stability, narrow molecular weight distribution and high production efficiency.

Active Publication Date: 2022-08-05
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In the existing literature, batch or continuous methods can be used to produce MQ resins, and there are also literature reports that modify MQ resins to improve their application range, but they have not discussed how to produce MQ resins with narrow molecular weight distribution.

Method used

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  • A kind of preparation method of mq resin with narrow molecular weight distribution
  • A kind of preparation method of mq resin with narrow molecular weight distribution
  • A kind of preparation method of mq resin with narrow molecular weight distribution

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] At 15°C, 40w.t.% aqueous sodium silicate solution (modulus 3.1) and 20w.t.% aqueous hydrochloric acid were mixed according to SiO 2 / HCl molar ratio = 0.5 to carry out the reaction. The static mixer in the reactor A is a SK type static mixer, the number of units is 20, the liquid flow rate is 5m / s, and the residence time is 0.4s. The aging reactor in Reactor A is a tubular reactor with a residence time of 30 min.

[0046] The product, isopropanol, hexamethyldisiloxane, trimethylchlorosilane, polyether silicone oil (molecular weight 2000, HLB value 1.5) in reactor A were 87.75kg / h, 20.25kg / h, 20.25 kg / h, 6.075kg / h, 0.675kg / h were continuously added to Reactor B. The reaction temperature of the reactor B was 80° C., the reaction pressure was 1 bar, and the end-capping reaction time was 120 min. The product of reactor B was sent to the continuous phase separator, and the residence time of the phase separator was 50 min. Finally, the organic phase separated by the phase...

Embodiment 2

[0048] At 30°C, 40w.t.% aqueous sodium silicate solution (modulus 3.1) and 20w.t.% aqueous hydrochloric acid were combined according to SiO 2 / HCl molar ratio = 0.6 to carry out the reaction. The static mixer in the reactor A is a SH type static mixer, the number of units is 10, the liquid flow rate is 8m / s, and the residence time is 0.125s. The aging reactor in Reactor A is a tubular reactor with a residence time of 20 min.

[0049] The product in reactor A, isopropanol, xylene, trimethylchlorosilane, vinyldimethylchlorosilane, polyether silicone oil (molecular weight 4000, HLB value 5) were respectively 87.75kg / h and 13.5kg / h. h, 13.5kg / h, 10kg / h, 9.57kg / h, 0.675kg / h were continuously added to reactor B. The reaction temperature of the reactor B was 70° C., the reaction pressure was 0.1 bar, and the end-capping reaction time was 180 min. The product of reactor B was sent to the continuous phase separator, and the residence time of the phase separator was 20 min. Finally,...

Embodiment 3

[0051] At 0°C, 40w.t.% aqueous sodium silicate solution (modulus 3.1) and 20w.t.% aqueous hydrochloric acid were combined according to SiO 2 / HCl molar ratio = 0.8 to carry out the reaction. The static mixer in the reactor A is a SL type static mixer, the number of units is 30, the liquid flow rate is 3m / s, and the residence time is 1s. The aging reactor in Reactor A is a tubular reactor with a residence time of 120 min.

[0052] The product, ethanol, toluene, hexamethyldisiloxane and polyether silicone oil (molecular weight 1000, HLB value 1) in reactor A were 87.75kg / h, 20.25kg / h, 13.5kg / h, 13.36kg respectively. / h, 0.135 kg / h was continuously added to reactor B. The reaction temperature of the reactor B was 110° C., the reaction pressure was 3 bar, and the end-capping reaction time was 30 min. The product of reactor B was sent to the continuous phase separator, and the residence time of the phase separator was 100 min. Finally, the organic phase separated by the phase s...

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Abstract

The present invention provides a method for preparing MQ resin with narrow molecular weight distribution, comprising the following steps: a) continuous polymerization of sodium silicate and aqueous hydrochloric acid in reactor A to form polysilicic acid hydrosol; b) in reactor B In, adopt reactor A product, alcohol, solvent, capping agent, organosilicon additive to carry out capping reaction continuously; c) Reactor B product is divided into two phases: the organic phase and aqueous phase that comprise MQ resin; d) The organic phase containing the MQ resin is purified into a single solvent system MQ resin product by a continuous distillation process. The MQ resin of the present invention has the characteristics of continuous production and narrow molecular weight distribution.

Description

technical field [0001] The present invention relates to a preparation method of silicone resin, in particular to a preparation method of MQ resin with narrow molecular weight distribution. Background technique [0002] Silicone resins are a class of low molecular weight polymers with a three-dimensional network structure. According to its structural characteristics, it can be applied to many fields, such as adhesives, defoaming agents, additives, personal care, etc. [0003] MQ resins are a special class of silicone resins that have monovalent trimethylsilyl (M) units and tetravalent (Q) units. The Q unit in MQ resin is usually provided by sodium silicate or silicate. According to the different raw materials, the MQ resin process can be divided into sodium silicate method and silicate ester method. Among them, sodium silicate is widely used in the production of MQ resin due to its low cost. [0004] US published patent US3772247 provides a synthetic method for preparing M...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/04C08G77/06C08G77/46
CPCC08G77/04C08G77/06C08G77/46
Inventor 曹骏纪学顺孙家宽马伟封玲珑刘志锋马岩龙邵仁龙何东荣
Owner WANHUA CHEM GRP CO LTD