阅读说明：本技术 一种湿磨剥壳微蒸促溶的高浓水玻璃制备方法 (Preparation method of high-concentration water glass for wet grinding, husking and micro-steaming dissolution promotion ) 是由 宫志群 马占国 王凡 姬永生 胡煜松 龚鹏 张亮亮 严鹏飞 于 2021-09-16 设计创作，主要内容包括：本发明公开了一种湿磨剥壳微蒸促溶的高浓水玻璃制备方法,主要涉及水玻璃生产技术领域；包括步骤：S1、湿磨：以碱液作为溶剂,常温下将高硅质材料微粉湿磨成纳米胶体颗粒,从而形成浑浊粘稠的乳浊液；S2、微蒸：将乳浊液送至蒸压釜中微蒸制得澄清透明的高浓水玻璃；本发明能够在降低设备投资成本的前提下大幅度减少能耗,并实现硅质材料中非晶态硅质成分的高效溶出,最大程度提高生产效率,解决了现今水玻璃制法硅质成分溶出效率低和能耗过高的难题。(The invention discloses a preparation method of wet-milling husking micro-steaming dissolution-promoting high-concentration water glass, which mainly relates to the technical field of water glass production; the method comprises the following steps: s1, wet grinding: wet grinding the high-silicon material micro powder into nano colloidal particles at normal temperature by taking alkali liquor as a solvent, thereby forming turbid and viscous emulsion; s2, micro-steaming: sending the emulsion into a still kettle for micro-steaming to obtain clear and transparent high-concentration water glass; the invention can greatly reduce energy consumption on the premise of reducing equipment investment cost, realize high-efficiency dissolution of amorphous silicon components in the silicon material, improve production efficiency to the greatest extent and solve the problems of low dissolution efficiency and overhigh energy consumption of the silicon components prepared by the existing water glass method.)

1. A preparation method of wet-milling husking micro-steaming dissolution-promoting high-concentration water glass is characterized by comprising the following steps:

s1, wet grinding: wet grinding the high-silicon material micro powder into nano colloidal particles at normal temperature by taking alkali liquor as a solvent, thereby forming turbid and viscous emulsion;

s2, micro-steaming: and (4) sending the emulsion into a still kettle for micro-steaming to obtain clear and transparent high-concentration water glass.

2. The method for preparing the high-concentration water glass for wet grinding, husking and micro-steaming dissolution promotion according to claim 1, wherein the method comprises the following steps: in the step S1, 25-40% of the high-silicon material micro powder and 60-75% of the alkali liquor.

3. The method for preparing the high-concentration water glass for wet grinding, husking and micro-steaming dissolution promotion according to claim 1, wherein the method comprises the following steps: in step S1, the high-silicon material is a silicon component SiO₂Material in an amount of not less than 95% wt.

4. The method for preparing the high-concentration water glass for wet grinding, husking and micro-steaming dissolution promotion according to claim 1, wherein the method comprises the following steps: in the step S1, the alkali liquor is NaOH or KOH solution with the concentration of 20-50%.

5. The method for preparing the high-concentration water glass for wet grinding, husking and micro-steaming dissolution promotion according to claim 1, wherein the method comprises the following steps: in the step S1, the high-silicon material micro powder is prepared by grinding high-silicon material powder into powder with specific surface area not less than 600m²Powder of/kg.

6. The method for preparing the high-concentration water glass for wet grinding, husking and micro-steaming dissolution promotion according to claim 1, wherein the method comprises the following steps: in step S1, the wet grinding is to wet grind the high-siliceous material micropowder in alkaline solution until the high-siliceous material micropowder is fully dissolved into a homogeneous viscous liquid state.

7. The method for preparing the high-concentration water glass for wet grinding, husking and micro-steaming dissolution promotion according to claim 1, wherein the method comprises the following steps: in the step S2, the steaming and pressing system of the micro-steaming is as follows: the temperature is 110-.

8. The method for preparing the high-concentration water glass for wet grinding, husking and micro-steaming dissolution promotion according to claim 1, wherein the method comprises the following steps: in the step S2, the clear transparent high-concentration water glass is a water glass colloidal solution with a Baume degree of 30-50 and a modulus of 1.5-3.3.

Technical Field

The invention relates to the technical field of water glass production, in particular to a preparation method of high-concentration water glass for wet grinding, husking and micro-steaming dissolution promotion.

Background

The water glass is the water solution of sodium silicate, and the production process includes a dry method and a wet method. According to the dry method, quartzite and soda ash are used as raw materials, and the solid sodium silicate is prepared by calcining the raw materials in a kiln at the high temperature of 1300-1500 ℃ for 4-6 hours. The solid sodium silicate has no use function in the actual industry, is only in a transition state, and is added into a dissolving roller according to the specified proportion according to the actual production process requirement, then steam is filled into the dissolving roller, and the dissolving roller reacts for 4 to 6 hours under the conditions of heating (150 to 170 ℃) and pressurizing (0.5 to 0.8MPa) to generate water glass with different concentrations and different moduli. The material melting process needs stirring and pressurization, and a drum-type reaction kettle or a static pressure type reaction kettle with a stirring device is generally adopted. The process has the advantages that the concentration and the modulus of the produced water glass are easy to adjust, but the calcining energy consumption of the kiln is too high, the sulfur-containing waste gas generated in the production has great pollution to the environment, and the liquid water glass can be obtained only by a two-step method, so the production efficiency is low.

The wet-process water glass production process takes quartz sand with the siliceous content not lower than 97 percent and liquid caustic soda with the concentration not lower than 32 percent as raw materials, and the raw materials are mixed according to the weight ratio of 1: putting the mixture into a drum-type sodium silicate device according to the proportion of 1.5, then filling steam, and keeping the mixture in rotation reaction for 10 hours under the conditions of heating (170-220 ℃) and pressurizing (1-2 MPa), so as to directly generate the low-modulus liquid water glass between 2.0 and 2.5. Although the method omits the calcining step of a kiln, the raw materials need to be autoclaved for a long time under the conditions of high temperature and high pressure, so that the energy consumption is still overhigh. Meanwhile, the high-pressure reaction has larger abrasion to equipment, and common equipment is difficult to be qualified, so that the requirement on the equipment is strict, namely thicker plates, such as drum-type sodium silicate equipment, need to be prepared, and the cost investment is increased.

From the perspective of preparation cost, safety and environmental protection, the processing method with low energy consumption, low pollution and high production efficiency is undoubtedly the development trend of water glass preparation in the future. Therefore, the preparation method for the water glass capable of producing different moduli and having low energy consumption, low equipment requirement and high production efficiency is searched to meet the application requirements of more industries, and has very important significance.

Disclosure of Invention

The invention aims to solve the problems in the prior art and provides a method for preparing high-concentration water glass by wet grinding, husking and micro-steaming dissolution promotion.

In order to achieve the purpose, the invention is realized by the following technical scheme:

a preparation method of wet-milling husking micro-steaming dissolution-promoting high-concentration water glass comprises the following steps:

s1, wet grinding: wet grinding the high-silicon material micro powder into nano colloidal particles at normal temperature by taking alkali liquor as a solvent, thereby forming turbid and viscous emulsion;

s2, micro-steaming: and (4) sending the emulsion into a still kettle for micro-steaming to obtain clear and transparent high-concentration water glass.

Preferably, in the step S1, 25-40% of the high-siliceous material micro powder and 60-75% of the alkali solution are mixed, and the water glass solutions with different moduli and different baume degrees can be obtained by adjusting the mixing ratio of the alkali solution and the high-siliceous material, so as to meet the requirements of different industries on water glass.

Preferably, in step S1, the high-siliceous material is a siliceous component SiO₂The material with the content not less than 95 percent by weight can adopt quartz sand, silica fume and the like.

Preferably, in step S1, the alkali solution is 20% to 50% NaOH or KOH solution.

Preferably, in step S1, the high-silicon material micro powder is prepared by grinding high-silicon material powder into powder with specific surface area not less than 600m²Powder of/kg.

Preferably, in step S1, the wet grinding is to wet grind the high-siliceous material micropowder in alkaline solution until the high-siliceous material micropowder is fully dissolved into a homogeneous viscous liquid state.

Preferably, in step S2, the autoclaving system of the micro-steaming is: the temperature is 110-. The nano colloidal particles in the emulsion prepared by wet grinding under the autoclave system can be fully dissolved to form clear and transparent high-concentration water glass solution.

Preferably, in the step S2, the clear transparent high-concentration water glass is a water glass colloidal solution with a baume degree of 30-50 and a modulus of 1.5-3.3.

Compared with the prior art, the invention has the beneficial effects that:

1. the invention can realize the high-efficiency dissolution of the amorphous silicon component in the silicon material;

the traditional water glass preparation method needs to keep the raw materials under the conditions of heating and high pressure for a long time to carry out rotation reaction, so that the dissolution of amorphous silicon components in the silicon material can be promoted, and the production efficiency is low; in the invention, alkali liquor is used as a solvent, and the high-silicon material micro powder is wet-milled into homogeneous viscous emulsion at normal temperature; in the wet grinding pretreatment process of the high-silicon material micro powder and alkali liquor, micro powder particles react with the alkali liquor violently, and are quickly peeled and disintegrated from the surface to the inside into nano-scale components with small sizes; emulsion after wet grinding only needs to be sent to a still kettle for micro-steaming, so that the rapid and complete dissolution of amorphous silicon components can be realized; the reaction speed is high, the product conversion rate is high, and high-concentration water glass with stable quality can be produced in a short time.

2. The invention can greatly reduce the energy consumption on the premise of reducing the equipment investment cost;

the high-silicon material micro powder used in the invention has the characteristic of high reaction activity after wet grinding pretreatment by alkali liquor, and can achieve the due reaction activity without calcining and activating the high-silicon material micro powder compared with a dry method, thereby saving the energy consumption in the calcining and activating process; meanwhile, the reaction time and temperature required by the micro-evaporation are relatively less, and the preparation of the water glass can be finished after the reaction is carried out at the temperature of 110-130 ℃ for 0.5-2 h. Compared with the traditional wet method, the method has the advantages that the quartz sand and the sodium carbonate are kept in rotation reaction for 10 hours at high temperature (170-220 ℃) to prepare the water glass, and the energy consumption in the steam pressure reaction process is greatly reduced.

According to the invention, only a small-amplitude pressurization (0.2-0.5 Mpa) reaction is needed in the process of preparing the water glass, and compared with the traditional wet method, the water glass with the modulus not higher than 2.5 can be obtained in a high-pressure environment (pressurization of 2-3 Mpa), so that the abrasion to equipment is greatly reduced, the equipment investment cost is reduced, and the operation danger is avoided.

Drawings

FIG. 1 is a schematic mechanism of the wet milling, husking and micro-steaming dissolution promotion preparation of high-concentration water glass by taking single high-siliceous material micro-powder particles as an example;

FIG. 2 is a schematic diagram of a mechanism for preparing water glass by a conventional wet method by taking a single quartz particle as an example.

Detailed Description

The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and these equivalents also fall within the scope of the present application.

Example 1:

300 parts by weight of 98% SiO₂Sending 800 parts by weight of 30% NaOH solution containing silica fume into a wet grinder, and carrying out wet grinding for 1h at the rotating speed of 220r/min to obtain turbid and viscous emulsion 1.

And (3) feeding the emulsion 1 into a still kettle, and introducing water vapor into the still kettle to directly heat. Pressurizing the kettle at 0.4MPa and controlling the temperature at 120 ℃, and carrying out pressure-maintaining reaction for 1.5h to obtain the clear and transparent high-concentration water glass 1.

SiO in the high-concentration water glass 1 by silicon-molybdenum-blue spectrophotometric analysis₂13.50% (wt), modulus 3.3, SiO in silica fume₂The dissolution rate of (A) was 92.4%.

Example 2:

taking 300 parts by weight of 95% SiO₂The quartz sand with the content is ground into micro powder by a ball mill for 0.5h at the rotating speed of 190 r/min.

Feeding the quartz sand micro powder and 800 parts by weight of 30% NaOH solution into a wet grinding machine, and carrying out wet grinding for 1h at the rotating speed of 220r/min to obtain turbid and viscous emulsion 2.

And (3) feeding the emulsion 2 into a still kettle, and introducing water vapor into the still kettle to directly heat. Pressurizing the kettle at 0.5MPa and 130 ℃, and carrying out pressure-maintaining reaction for 2 hours to obtain the high-concentration water glass 2.

SiO in the high-concentration water glass 2 by silicon-molybdenum blue spectrophotometric analysis₂The content of SiO in the quartz sand is 12.90% (wt), the modulus is 3.1₂The dissolution rate was 88.6%.

The mechanism of wet grinding, husking and micro-steaming dissolution promotion of the invention is as follows:

the traditional wet method takes quartz sand and liquid caustic soda as raw materials, and can only generate liquid water glass with low modulus between 2.0 and 2.5 even if the rotary reaction is maintained for a long time under the condition of heating and high pressure. As shown in FIG. 2, the loose part of the surface layer reacts with the alkali solution to form flocculent colloid, which adheres to the surface of the quartz sand particles to form a thick coating layer, and the liquid water glass is slowly dissolved out along with the rotation of the autoclave. Until the coating layer is completely dissolved and falls off, the new exposed surface is continuously reacted with the alkali liquor, and the process is circulated to continuously generate a new flocculent colloid coating layer. And because the quartz sand particles are of a core-shell structure which tends to be more compact from the surface to the inside, the more viscous the coating layer formed by the reaction in the more inside is, the more difficult the coating layer is to dissolve and fall off. Therefore, the flocculent colloid coating layer is difficult to fall off and is continuously generated, which is a main cause of low dissolution efficiency of the siliceous component by the wet process.

The invention prepares the high-concentration water glass by carrying out wet grinding pretreatment on the alkali liquor of the high-silicon material micropowder and then carrying out micro-steaming, thereby really realizing the complete dissolution of the active silicon component. As shown in figure 1, the high siliceous material micropowder particles are rapidly stripped once the flocculent colloid coating layer adhered to the surface of the high siliceous material micropowder particles is generated through reaction under the action of huge energy generated by alkali liquid wet grinding, and then the high siliceous material micropowder particles are wet-ground into finer nanoscale components under the synergistic action of alkali liquid excitation and a grinding medium. While the coating layer is continuously stripped, the inner core with extremely high silicon content in the micro powder particle is also ground into the silicon nano particle with small size, and the silicon nano particle is endowed with extremely high silicon component dissolving activity. Only by giving the micro-steaming condition to the viscous mixed liquid after wet grinding, the nano-scale flocculent colloid and the amorphous siliceous component in the siliceous nano particles can be promoted to be completely dissolved out and rapidly and violently react with the alkali liquor under the heating condition to generate the liquid high-concentration water glass.