阅读说明：本技术 一种环保有机硅新材料及其制备方法 (Novel environment-friendly organic silicon material and preparation method thereof ) 是由 吴秀梅 王素珍 于 2021-01-09 设计创作，主要内容包括：本发明提供一种环保有机硅新材料及其制备方法,涉及有机硅制取技术领域。包括以下步骤：步骤一：原料准备：在热熔的铁矿石中投入适量的石灰石和化渣剂,对产生的硅酸钙进行粉碎待用,硅酸钙与硫酸钠混合,随后灼烧硅酸钙溶液生产二氧化硅、再次粉碎待用,步骤二：原料处理：二氧化硅通入氯气和焦炭,通过反应釜制取氯化硅,随后氯化硅原料与氢气反应制取粗硅。通过炼钢时,投入的石灰石所产生的硅酸钙进行收集在利用,可以进一步提高对废弃物的再次利用效率,避免产生资源的浪费,其次通过大量制备硅粉,可以提高整体反应的制备效率,加入过量硅粉,可以进一步提高制备量,避免产量不足导致的生产效益不佳的问题。(The invention provides a novel environment-friendly organic silicon material and a preparation method thereof, and relates to the technical field of organic silicon preparation. The method comprises the following steps: the method comprises the following steps: preparing raw materials: adding a proper amount of limestone and a slag melting agent into hot-melt iron ore, crushing the generated calcium silicate for later use, mixing the calcium silicate with sodium sulfate, then firing a calcium silicate solution to produce silicon dioxide, and crushing again for later use, wherein the second step is as follows: raw material treatment: introducing chlorine and coke into the silicon dioxide, preparing silicon chloride by a reaction kettle, and then reacting the silicon chloride raw material with hydrogen to prepare crude silicon. During through the steelmaking, the produced calcium silicate of lime stone that drops into is collected and is being utilized, can further improve the reuse efficiency to the discarded object, avoids producing the waste of resource, secondly through preparing silica flour in a large number, can improve the preparation efficiency of whole reaction, adds excessive silica flour, can further improve the preparation volume, avoids the not good problem of productivity effect that the output is not enough to lead to.)

1. The new environment-friendly organic silicon material and the preparation method thereof are characterized by comprising the following steps:

the method comprises the following steps: preparing raw materials: adding a proper amount of limestone and a slag melting agent into hot-melt iron ore, crushing the generated calcium silicate for later use, mixing the calcium silicate with sodium sulfate, then firing a calcium silicate solution to produce silicon dioxide, and crushing again for later use;

step two: raw material treatment: introducing chlorine and coke into the silicon dioxide, preparing silicon chloride through a reaction kettle, reacting the silicon chloride raw material with hydrogen to prepare crude silicon, and crushing for later use;

step three: production reaction: methyl chloride and silicon powder are directly synthesized in one step under the catalysis of cuprous chloride to generate a methyl chlorosilane mixture;

step four: purification and preparation: the methyl chlorosilane mixture is arranged in distillation purification equipment to be removed;

step five: and (3) preparing a finished product: and (3) carrying out mixing reaction on methyl chlorosilane, a solvent and an acrylic resin polymerization monomer to finally prepare the organic silicon modified acrylic resin.

2. The new environment-friendly organic silicon material and the preparation method thereof as claimed in claim 1, characterized by comprising the following steps: according to the operation step in the first step, the components of the slagging agent comprise aluminum compounds and iron oxide, the calcium silicate is crushed for standby application, and the diameter of the calcium silicate is less than 2 mm.

3. The new environment-friendly organic silicon material and the preparation method thereof as claimed in claim 1, characterized by comprising the following steps: according to the operation steps in the first step, mixing the calcium silicate and the sodium sulfate to prepare water glass by adopting a reaction kettle, then mixing the diluted water glass and dilute sulfuric acid at 20-30 ℃ to react to prepare silica gel, aging for 4h, soaking for 1h by using 2-2.5% dilute sulfuric acid, washing by using 40-50 ℃ water, dehydrating in a rotary drum dryer until the water content is less than or equal to 80%, drying until the water content is less than or equal to 10%, and placing in an activation furnace at 500-550 ℃ for activation to finally prepare the silicon dioxide.

4. The new environment-friendly organic silicon material and the preparation method thereof as claimed in claim 1, characterized by comprising the following steps: according to the operation steps in the second step, the actual introduction ratio of chlorine and coke introduced into the silicon dioxide is 1: 2: 1.

5. the new environment-friendly organic silicon material and the preparation method thereof as claimed in claim 1, characterized by comprising the following steps: according to the operation step in the second step, the coarse silicon is crushed to ensure that the particle diameter is less than 2 mm.

6. The new environment-friendly organic silicon material and the preparation method thereof as claimed in claim 1, characterized by comprising the following steps: according to the operation steps in the third step, the reaction temperature of the methane and the silicon powder in the catalysis of the cuprous chloride is 300-500 ℃.

7. The new environment-friendly organic silicon material and the preparation method thereof as claimed in claim 1, characterized by comprising the following steps: according to the operation steps in the third step, the methyl chlorosilane mixture is prepared and then stored at 15 ℃.

8. The new environment-friendly organic silicon material and the preparation method thereof as claimed in claim 1, characterized by comprising the following steps: according to the operation step in the fourth step, the distillation temperature of the mixture of methylchlorosilanes is 65 ℃.

9. The new environment-friendly organic silicon material and the preparation method thereof as claimed in claim 1, characterized by comprising the following steps: according to the operation steps in the fourth step, the purified mixture is stored for later use, and the storage temperature is 15 ℃.

10. The new environment-friendly organic silicon material and the preparation method thereof as claimed in claim 1, characterized by comprising the following steps: according to the operation steps in the fifth step, the methyl chlorosilane firstly reacts with the acrylic resin polymerization monomer, and then reacts with the acrylic resin polymer, wherein the acrylic resin polymerization monomer is in an excessive input state.

Technical Field

The invention relates to the technical field of organic silicon preparation, in particular to a novel environment-friendly organic silicon material and a preparation method thereof.

Background

Because of the unique structure of the organic silicon, the organic silicon has the performances of inorganic materials and organic materials, has the basic properties of low surface tension, small viscosity-temperature coefficient, high compressibility, high gas permeability and the like, and has the excellent characteristics of high and low temperature resistance, electrical insulation, oxidation resistance stability, weather resistance, flame retardancy, hydrophobicity, corrosion resistance, no toxicity, no odor, physiological inertia and the like, is widely applied to the industries of aerospace, electronics and electricity, construction, transportation, chemical industry, textile, food, light industry, medical treatment and the like, the organic silicon is mainly applied to sealing, bonding, lubricating, coating, surface activity, demoulding, defoaming, foam inhibition, water prevention, moisture prevention, inert filling and the like, the application field is continuously widened along with the continuous increase of the number and varieties of the organic silicon, a unique important product system in a new chemical material field is formed, and a plurality of varieties are indispensable and cannot be replaced by other chemicals.

At present, the three-proofing glue generated by organosilane is limited by the yield of organosilane, so that in the actual production process, most of the cost is controlled in the utilization of effective components, silicon powder is prepared independently, the actual environmental protection efficiency is poor, calcium silicate generated in steel making cannot be well applied, the existing three-proofing glue is poor in environmental protection performance, the actual preparation efficiency is poor due to the limitation of yield, and the economic benefit is not obviously reduced.

Disclosure of Invention

The invention aims to provide a novel environment-friendly organic silicon material and a preparation method thereof. During through the steelmaking, the produced calcium silicate of lime stone that drops into is collected and is being utilized, can further improve the reuse efficiency to the discarded object, avoids producing the waste of resource, secondly through preparing silica flour in a large number, can improve the preparation efficiency of whole reaction, adds excessive silica flour, can further improve the preparation volume, avoids the not good problem of productivity effect that the output is not enough to lead to.

In order to solve the problems of poor environment-friendly performance and low structural strength, the invention provides the following technical scheme: an environment-friendly organic silicon new material and a preparation method thereof comprise the following steps:

the method comprises the following steps: preparing raw materials: adding a proper amount of limestone and a slag melting agent into hot-melt iron ore, crushing the generated calcium silicate for later use, mixing the calcium silicate with sodium sulfate, then firing a calcium silicate solution to produce silicon dioxide, and crushing again for later use.

Step two: raw material treatment: introducing chlorine and coke into the silicon dioxide, preparing silicon chloride through a reaction kettle, reacting the silicon chloride raw material with hydrogen to prepare crude silicon, and crushing for later use.

Step three: production reaction: methyl chloride and silicon powder are directly synthesized in one step under the catalysis of cuprous chloride to generate a methyl chlorosilane mixture.

Step four: purification and preparation: and (3) setting the methyl chlorosilane mixture into distillation purification equipment for removing.

Step five: and (3) preparing a finished product: and (3) carrying out mixing reaction on methyl chlorosilane, a solvent and an acrylic resin polymerization monomer to finally prepare the organic silicon modified acrylic resin.

Further, according to the operation step in the first step, the components of the slagging agent comprise aluminum compounds and iron oxide, the calcium silicate is crushed for standby, and the diameter of the calcium silicate is less than 2 mm.

Further, according to the operation steps in the step one, the calcium silicate and the sodium sulfate are mixed to prepare water glass by adopting a reaction kettle, then the diluted water glass and dilute sulfuric acid are mixed at 20-30 ℃ to react to prepare silica gel, the silica gel is aged for 4h, soaked for 1h by using 2-2.5% dilute sulfuric acid, washed by using 40-50 ℃ water, dehydrated in a rotary drum dryer until the water content is less than or equal to 80%, dried until the water content is less than or equal to 10%, placed in an activation furnace at 500-550 ℃ to be activated, and finally the silicon dioxide is prepared.

Further, according to the operation steps in the second step, the actual introduction ratio of chlorine gas and coke introduced into the silica is 1: 2: 1.

further, according to the operation step in the second step, the pulverization of the crude silicon ensures that the particle diameter is less than 2 mm.

Further, according to the operation steps in the third step, the reaction temperature of the methane and the silicon powder under the catalysis of the cuprous chloride is 300-500 ℃.

Further, according to the operation steps in the third step, the methyl chlorosilane mixture is prepared and then stored at 15 ℃.

Further, according to the operation steps in the fourth step, the distillation temperature of the mixture of methylchlorosilanes is 65 ℃.

Further, according to the operation steps in the fourth step, the purified mixture is stored for later use, and the storage temperature is 15 ℃.

Further, according to the operation steps in the fifth step, the methylchlorosilane is reacted with the acrylic resin polymerization monomer, and then reacted with the acrylic resin polymer, wherein the acrylic resin polymerization monomer is in an excessive input state.

The invention provides an environment-friendly organic silicon new material and a preparation method thereof, and the environment-friendly organic silicon new material has the following beneficial effects: during through the steelmaking, the produced calcium silicate of lime stone that drops into is collected and is being utilized, can further improve the reuse efficiency to the discarded object, avoids producing the waste of resource, secondly through preparing silica flour in a large number, can improve the preparation efficiency of whole reaction, adds excessive silica flour, can further improve the preparation volume, avoids the not good problem of productivity effect that the output is not enough to lead to.

Drawings

FIG. 1 is a flow chart of a new environment-friendly organic silicon material and a preparation method thereof.

Detailed Description

Referring to fig. 1, the present invention provides a technical solution: an environment-friendly organic silicon new material and a preparation method thereof comprise the following steps:

the method comprises the following steps: preparing raw materials: adding a proper amount of limestone and a slag melting agent into hot-melt iron ore, crushing the generated calcium silicate for later use, mixing the calcium silicate with sodium sulfate, then firing a calcium silicate solution to produce silicon dioxide, and crushing again for later use.

Step two: raw material treatment: introducing chlorine and coke into the silicon dioxide, preparing silicon chloride through a reaction kettle, reacting the silicon chloride raw material with hydrogen to prepare crude silicon, and crushing for later use.

Step three: production reaction: methyl chloride and silicon powder are directly synthesized in one step under the catalysis of cuprous chloride to generate a methyl chlorosilane mixture.

Step four: purification and preparation: and (3) setting the methyl chlorosilane mixture into distillation purification equipment for removing.

Step five: and (3) preparing a finished product: and (3) carrying out mixing reaction on methyl chlorosilane, a solvent and an acrylic resin polymerization monomer to finally prepare the organic silicon modified acrylic resin.

Specifically, according to the operation steps in the step one, the components of the slagging agent comprise aluminum compounds and iron oxide, calcium silicate is crushed for standby, and the diameter of the calcium silicate is less than 2 mm.

Specifically, according to the operation steps in the step one, mixing calcium silicate and sodium sulfate is prepared into water glass by using a reaction kettle, then the diluted water glass and dilute sulfuric acid are mixed at 20-30 ℃ to react to prepare silica gel, aging is carried out for 4h, the silica gel is soaked for 1h by using 2-2.5% dilute sulfuric acid, washing is carried out by using 40-50 ℃ water, dehydration is carried out in a rotary drum dryer until the water content is less than or equal to 80%, the silica gel is dried until the water content is less than or equal to 10%, and the silica gel is placed in an activation furnace at 500-550 ℃ to be activated to finally prepare the silica.

Specifically, according to the operation steps in the second step, the actual introduction ratio of chlorine to coke into the silica is 1: 2: 1.

specifically, according to the operation step in the second step, the pulverization of the crude silicon ensures that the particle diameter is less than 2 mm.

Specifically, according to the operation steps in the third step, the reaction temperature of the methane and the silicon powder under the catalysis of the cuprous chloride is 300-500 ℃.

Specifically, according to the operation steps in the third step, the methyl chlorosilane mixture is prepared and then stored at 15 ℃.

Specifically, according to the operation steps in the fourth step, the distillation temperature of the mixture of methylchlorosilanes was 65 ℃.

Specifically, according to the operation steps in the fourth step, the purified mixture is stored for later use, and the storage temperature is 15 ℃.

Specifically, according to the operation steps in the fifth step, the methylchlorosilane is reacted with the acrylic resin polymerization monomer first, and then reacted with the acrylic resin polymer, and the acrylic resin polymerization monomer is in an excessive input state.

The method of the examples was performed for detection analysis and compared to the prior art to yield the following data:

	efficiency of environmental protection	Efficiency of preparation
			Examples	Is higher than	Is higher than
Prior Art	Is lower than	Is lower than

According to the table data, when the embodiment is used, the stable utilization of the by-products of other processes is further improved and the overall preparation efficiency is improved through the novel environment-friendly organic silicon material and the preparation method thereof.

The invention provides an environment-friendly organic silicon new material and a preparation method thereof, wherein the preparation method comprises the following steps: the method comprises the following steps: preparing raw materials: adding a proper amount of limestone and a slag melting agent into hot-melt iron ore, crushing the generated calcium silicate for standby use, mixing the calcium silicate with sodium sulfate, then firing a calcium silicate solution to produce silicon dioxide, crushing the mixture for standby use again, wherein the components of the slag melting agent comprise an aluminum compound and iron oxide, crushing the calcium silicate for standby use, the diameter of the calcium silicate is less than 2 mm, preparing water glass by mixing the calcium silicate with the sodium sulfate in a reaction kettle, then mixing the diluted water glass with dilute sulfuric acid at 20-30 ℃ for reaction to prepare silica gel, aging the silica gel for 4h, soaking the silica gel for 1h by using 2-2.5% of dilute sulfuric acid, washing the silica gel by using 40-50 ℃ water, dehydrating the silica gel in a rotary drum dryer until the water content is less than or equal to 80%, drying the silica gel until the water content is less than or equal to 10%, placing the silica gel in an activation furnace at 500-550 ℃ for activation, finally, step two: raw material treatment: silica lets in chlorine and coke, prepares silicon chloride through reation kettle, and the crude silicon is prepared with hydrogen reaction to the silicon chloride raw materials afterwards, smashes the back for use, through crude silicon, can realize the quick preparation to silica flour, improves the preparation volume of methyl chlorosilane, and the actual proportion of letting in that silica lets in chlorine and coke is 1: 2: 1, coke can be used as an efficient reducing agent, the particle diameter of coarse silicon is ensured to be less than 2 mm by crushing, and the step three is as follows: production reaction: directly synthesizing chloromethane and silicon powder in the one step under the catalysis of cuprous chloride to generate a methyl chlorosilane mixture, storing the prepared methyl chlorosilane mixture at 15 ℃, and keeping the reaction temperature of the methane and the silicon powder at 300-500 ℃ under the catalysis of the cuprous chloride, wherein the fourth step is as follows: purification and preparation: setting the methyl chlorosilane mixture into distillation and purification equipment to be removed, wherein the distillation temperature of the methyl chlorosilane mixture is 65 ℃, the pure mixture is stored for later use, the storage temperature is 15 ℃, and the fifth step is as follows: and (3) preparing a finished product: the preparation method comprises the following steps of carrying out mixed reaction on methyl chlorosilane, a solvent and an acrylic resin polymerized monomer to finally prepare the organic silicon modified acrylic resin, wherein the methyl chlorosilane firstly reacts with the acrylic resin polymerized monomer and then reacts with an acrylic resin polymer, the acrylic resin polymerized monomer is in an excessive input state, stable buffering can be realized for the reaction through the solvent, and the solvent adopts 1: 1: 1 mixing the solvent.

Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.