CN103265045A - Method for producing potassium silicate solution for electronic industry - Google Patents
Method for producing potassium silicate solution for electronic industry Download PDFInfo
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- CN103265045A CN103265045A CN2013102157760A CN201310215776A CN103265045A CN 103265045 A CN103265045 A CN 103265045A CN 2013102157760 A CN2013102157760 A CN 2013102157760A CN 201310215776 A CN201310215776 A CN 201310215776A CN 103265045 A CN103265045 A CN 103265045A
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Abstract
The invention discloses a method for producing a potassium silicate solution for the electronic industry. The potassium silicate solution is prepared by reacting high-purity ultra-fine silicon micro powder and a potassium hydroxide solution which serve as raw materials. The method comprises the following steps of: diluting the potassium hydroxide solution produced by an ionic membrane method to 20-25 percent, stirring the raw materials, raising the temperature to 80 DEG C, slowly adding the high-purity ultra-fine silicon micro powder, continuously raising the temperature to 95-100 DEG C, stirring the materials by preserving the temperature for 1 hour, detecting a sample, adjusting a die, after a modulus is qualified, diluting the solution to required concentration by electronic-level pure water, and stirring the materials for 20 minutes to obtain the potassium silicate solution for the electronic industry. The method is simple, practical, quick, convenient, energy-saving, environment-friendly, low-carbon and clean; and the product potassium silicate solution can meet the GB/T9394-1998 standard requirement.
Description
Technical field
The invention belongs to the production method of potassium silicate solution, be specifically related to a kind of production method of used in electronic industry potassium silicate solution.
Background technology
Used in electronic industry potassium silicate solution (GB/T9394-1998) is mainly used in electron tube fluorescence beam screen and applies, and also can be used as the subsidiary material of making fluorescent material and electrically conductive graphite breast.Its product the key technical indexes is: 1, outward appearance should not have mechanical impurity, and colourity is not deeper than standard No. 5, and turbidity is not more than the clarity standard No. 5; 2, potassium silicate massfraction (total alkalinity quality percentage composition and the silicon-dioxide quality percentage composition sum represented with potassium oxide) is 28% ± 0.5%; 3, modulus (ratio of silicon-dioxide and potassium oxide amount of substance in the potassium silicate) is 3.40 ± 0.03; 4, iron level (massfraction, down together)≤0.0003%; 5, copper content≤0.000001%; 6, nickel content :≤0.000005%; 7, heavy metal (in lead) content≤0.00005%; 8, cl content≤0.001%; 9, carbonate (in K2CO3)≤0.05%; 10, aluminium content is when customer requirements, by the mutual agreement regulation.
The production method of present used in electronic industry potassium silicate solution has three kinds: 1, ion exchange method: it is little that this method is subjected to the ion exchange resin exchange capacity to influence its output, the production cost height, and this method is superseded substantially now.2, wet production method: this ratio juris is to adopt water glass, nitric acid, potassium hydroxide to make raw material, utilize water glass and nitric acid reaction to make the silicon gel after rinsed with deionized water, adding the nitric acid acidifying purifies, post rinse is to neutral, make high-purity silicon dioxide after the centrifuge dehydration, make with the reaction of analytical pure potassium hydroxide again.This explained hereafter step complexity, production cycle length, nitric acid high volatility, pollute that production environment big, the workman is abominable, production cost is high, now do not have enterprise to adopt this method to produce.3, electric smelting method (dry method): this method is with used in electronic industry glass sand (SiO
2〉=99.90%, Fe≤8ppm; SiO
2〉=99.95%, Fe≤5ppm) and high-quality salt of wormwood or saleratus are raw material; SiO
2/ K
2CO
3(K
2HCO
3) carry out proportioning by certain amount of substance and join in the special-purpose electric smelting kiln, about 1100-1400 ℃, be melt into glass metal and flow out, can obtain the used in electronic industry potassium silicate solution with electron-grade water heating for dissolving, mode transfer, filtration again after the cooling.This method is the production method of the most frequently used used in electronic industry potassium silicate solution of present China, and ground producers such as Jiangsu, Hebei, Liaoning, Tianjin, Sichuan all adopt this method to produce.There is following insurmountable problem in this method when founding water pearl ash glass liquid: the interior nogging of (1), its electrode materials and kiln also can be corroded in this glass metal by water pearl ash glass liquid, will bring the contaminating impurity problem to product like this; (2), owing to adopt high-quality salt of wormwood or high quality carbon potassium hydrogen phthalate to make raw material and glass sand at high temperature takes place to emit carbon dioxide when physical-chemical reaction is produced water pearl ash glass liquid, this also can also bring pollution by environment; (3), owing to be high temperature melting, workman's operating environment is poor; (4), every production cycle of electric smelting kiln will overhaul or reconstruct, and increased production cost; (5), this solution moisture content height, transport to from manufactory and to use the merchant, increased transportation cost.
In order to solve the drawback of aforementioned production method, develop a kind of environmental friendliness, pollution-free, low-carbon (LC), moderate, the simple production method of used in electronic industry potassium silicate solution fast of cost, be one of important problem task of we silicon materials research staff.
Summary of the invention
Purpose of the present invention is exactly to overcome the problems referred to above that exist in the present used in electronic industry potassium silicate solution production method, and the production method of a kind of simple and practical, quick and convenient, energy-conserving and environment-protective, low-carbon (LC) cleaning, eco-friendly used in electronic industry potassium silicate solution is provided.
The production method of a kind of used in electronic industry potassium silicate solution of the present invention, the massfraction that requires its product mesosilicic acid potassium is 28% ± 0.5%, the ratio of silicon-dioxide and the amount of substance of potassium oxide in the potassium silicate, be that modulus n is 3.40 ± 0.03, it is characterized in that: be to be that raw material reaction makes with high pure and ultra-fine silicon powder and potassium hydroxide solution, comprise the steps:
(1) according to the total mass of the potassium silicate solution of required production, calculate the quality of required high pure and ultra-fine silicon powder and potassium hydroxide solution, basis:
NSiO
2+ 2KOH=K
2OnSiO
2+ H
2O, wherein n=3.40;
According to calculation result, accurately take by weighing required high pure and ultra-fine silicon powder and potassium hydroxide solution; SiO in the described high pure and ultra-fine silicon powder
2〉=99.98%, Fe≤2ppm, particle diameter are 0.5～5 micron; Described potassium hydroxide solution is that the massfraction of ionic membrane method production is 48% potassium hydroxide solution;
(2) potassium hydroxide solution that weighs up being added doing in the reactor of lining with polytetrafluoroethylmaterial material of band stirring, heating and temperature control unit, open whipping appts, is 20%～25% with an amount of electron-grade water dilute hydrogen potassium oxide solution to its massfraction;
(3) open heating, whipping appts, make reactor temperature reach 80 ℃, insulation slowly adds the high pure and ultra-fine silicon powder, behind reinforced the finishing, continues to heat up, and reaches 95～100 ℃, insulation reaction 1 hour to reactor temperature;
(4) sampling detects, modulus n according to the cubage potassium silicate solution of dioxide-containing silica and potassium oxide, if n=3.40 ± 0.03, then the product modulus is qualified, massfraction according to potassium silicate, adding an amount of electron-grade water, to be diluted to product mesosilicic acid potassium massfraction be 28%, stirred 20 minutes, namely; If following step (5) is carried out in n＞3.43; If following step (6) is carried out in n＜3.37;
(5) if the required quality of adding potassium hydroxide solution according to the n value, is calculated in n＞3.43, add required potassium hydroxide solution and stirred 20 minutes, sampling detects, repeating step (4);
(6) if the required quality of adding the high pure and ultra-fine silicon powder according to the n value, is calculated in n＜3.37, under agitation add the high pure and ultra-fine silicon powder and be warming up to 95～100 ℃, insulation reaction 30 minutes, sampling detects, repeating step (4).
Preferably, SiO in the used high pure and ultra-fine silicon powder among the present invention
2〉=99.98%, Fe≤2ppm, particle diameter is 0.5～5 micron, is to produce for the method for ZL201110247392.8 by Chinese invention patent number.Certainly this high pure and ultra-fine silicon powder also can be other commercially available like product, as long as SiO in its product
2〉=99.98%, particle diameter is 0.5～5 micron or thinner, namely can be used among the present invention.High-performances such as this high pure and ultra-fine silicon powder has the purity height, diameter of particle is trickle, specific surface area is big, high dielectric, high heat-resisting, high-temperature resistant, high filler loading capacity, low bulk, low-stress, low impurity, low-friction coefficient, especially it is soluble in potassium hydroxide solution, is particularly suitable for the present invention and prepares the used in electronic industry potassium silicate solution.
The used potassium hydroxide of the present invention is that the massfraction of ionic membrane method production is 48% potassium hydroxide solution, carries out and saves time for being conducive to reaction, and needing in the present invention earlier it is diluted to massfraction is 20%～25%.Because when the massfraction of potassium hydroxide solution is 25%～48%, material is too dense thick behind the adding high pure and ultra-fine silicon powder, is unfavorable for reacting and carries out, when the massfraction of potassium hydroxide solution is lower than 20%, potassium hydroxide solution concentration is too low, and speed of response is too slow, and length expends time in.
Reactor of the present invention is for making the reactor of lining with polytetrafluoroethylmaterial material, have characteristics such as strong alkali-acid resistance, high temperature resistant, resistance to oxidation, weather, radiation hardness, insulation, toxicological harmless, especially it has lubricated, the adhesion characteristics not of excellent height, make the present invention in the process of producing potassium silicate solution, do not have the contaminating impurity problem.
The present invention can also adopt another kind of method production, namely after weighing up required material, earlier the high pure and ultra-fine silicon powder is added in the reactor, and being mixed with massfraction with electron-grade water is 10%～20% SiO
2Slip adds massfraction and is 48% sodium hydroxide solution again, reacts 1～2 hour under 95～100 ℃ of conditions, detects in the potassium silicate solution the qualified back of modulus and adds electron-grade water and be diluted to desired concn and get final product.
With the used in electronic industry potassium silicate solution that the inventive method is produced, quality meets the GB/T9394-1998 standard.
The inventive method has the following advantages: (1) raw materials used marketable material that is, be convenient to buying and tissue is produced, and raw material is high purity grades, raw materials used and generate in the product and all do not have other foreign ions, chemical reaction only needs a step to finish, and can not introduce new contaminating impurity.(2) reaction vessel has been avoided the pollution that container brings product in the reaction process for make the reactor of liner with polytetrafluoroethylmaterial material.(3) technological process of production is simple, and reaction conditions is simple and easy to control, can organize production as required on the spot, has saved line-haul cost.
Embodiment
Embodiment 1
Be example to produce 700kg used in electronic industry potassium silicate solution, do 3 groups of parallel tests simultaneously, its product is designated as lot number 1, lot number 2, lot number 3, detects its repeatability.
(1) with potassium silicate solution mesosilicic acid potassium (K
2O3.4SiO
2) massfraction is 28% to do calculating, according to chemical equation: 3.4SiO
2+ 2KOH=K
2O3.4SiO
2+ H
2O calculates required high pure and ultra-fine silicon powder (SiO
2〉=99.98%, Fe≤2ppm, particle diameter are 0.5～5 micron) quality is 134.25kg, massfraction is that 48% KOH solution quality is 153.50kg, accurately takes by weighing high pure and ultra-fine silicon powder 134.25kg with electronic scale, 48% KOH solution 153.50 kg;
What (2) with the 153.50kg massfraction be that 48% KOH solution adds band stirring, heating and temperature control unit is in the 1000L reactor of lining with the tetrafluoroethylene, opening whipping appts, is 20% with 214.90kg electron-grade water dilute hydrogen potassium oxide solution to its massfraction;
(3) open heating, whipping appts, make reactor temperature reach 80 ℃, insulation slowly adds 134.25kg high pure and ultra-fine silicon powder, behind reinforced the finishing, continues to heat up, and reaches 95 ℃, insulation reaction 1 hour to reactor temperature;
(4) get the potassium silicate solution that makes in the step (3) and detect, detected result sees the following form:
Primary detection potassium silicate solution composition analysis table among table 1: the embodiment 1
% represents mass percent in the table, down together.
According to above-mentioned analysis, the product modulus is qualified, adds the 197.35kg electron-grade water, and restir 20 minutes namely obtains the used in electronic industry potassium silicate solution.Sampling inspection results sees the following form:
Table 2: embodiment 1 products obtained therefrom composition analysis table
Other foreign matter contents are in lot number 1～3 product: Fe≤0.0002%, Cu≤0.000001%, Ni≤0.000003%, Pb≤0.00005, Cl≤0.0005%, K
2CO
3≤ 0.03%.Product appearance is colourless transparent liquid.
Above-mentioned detected result explanation, the prepared used in electronic industry potassium silicate solution of present embodiment is qualified.
Embodiment 2
Be example to produce 750kg used in electronic industry potassium silicate solution, do 3 groups of parallel tests simultaneously, its product is designated as lot number 4, lot number 5, lot number 6, detects its repeatability.
(1) with potassium silicate solution mesosilicic acid potassium (K
2O3.4SiO
2) massfraction is 28% to do calculating, according to chemical equation: 3.4SiO
2+ 2KOH=K
2O3.4SiO
2+ H
2O; Calculate required high pure and ultra-fine silicon powder (SiO
2〉=99.98%, Fe≤2ppm, particle diameter are 0.5～5 micron) quality is 143.76kg, massfraction is that 48% KOH solution quality is 164.47kg, takes by weighing high pure and ultra-fine silicon powder 143.76kg with electronic scale, 48% KOH solution 164.47 kg;
What (2) with the 164.47kg massfraction be that 48% KOH solution adds band stirring, heating and temperature control unit is in the 1000L reactor of lining with the tetrafluoroethylene, opening whipping appts, is 25% with 151.29kg electron-grade water dilute hydrogen potassium oxide solution to its massfraction;
(3) open heating, whipping appts, make reactor temperature reach 80 ℃, insulation slowly adds 143.76kg high pure and ultra-fine silicon powder, behind reinforced the finishing, continues to heat up, and reaches 100 ℃, insulation reaction 1 hour to reactor temperature;
(4) get the potassium silicate solution that makes in the step (3) and detect, detected result sees Table 3:
Primary detection potassium silicate solution composition analysis table among table 3: the embodiment 2
According to above-mentioned detected result, the product modulus is qualified, adds the 290.48kg electron-grade water, and restir 20 minutes namely obtains the used in electronic industry potassium silicate solution.Sampling inspection results sees Table 4:
Table 4: embodiment 2 products obtained therefrom composition analysis tables
Other foreign matter contents are in lot number 4～6 products: Fe≤0.0002%, Cu≤0.000001%, Ni≤0.000003%, Pb≤0.00005, Cl≤0.0005%, K
2CO
3≤ 0.03%. product appearance is colourless transparent liquid.
Above-mentioned detected result explanation, the prepared used in electronic industry potassium silicate solution of present embodiment is qualified.
Embodiment 3
Be example to produce 700kg used in electronic industry potassium silicate solution, do 3 groups of parallel tests simultaneously, its product is designated as lot number 7, lot number 8, lot number 9.Preparation process (1)～(3) are with embodiment 1;
(4) get the potassium silicate solution that makes in the step (3) and detect, detected result sees Table 5:
Primary detection potassium silicate solution composition analysis table among table 5: the embodiment 3
According to above-mentioned analysis, lot number 8,9 product moduluses are qualified, add the 197.35kg electron-grade water, and restir 20 minutes namely obtains the used in electronic industry potassium silicate solution;
(5) lot number 7 product moduluses are defective, and as calculated, adding 2.43kg massfraction is 48% KOH solution, stirring reaction 20 minutes, and sampling inspection results is as follows:
Lot number: 7, SiO
2: 26.95%, K
2O:12.44%, concentration of potassium silicate (K
2OnSiO
2): 39.39%.n=3.40；
Modulus is qualified, adds the 205.46kg electron-grade water, and restir 20 minutes namely obtains the used in electronic industry potassium silicate solution.Lot number 7,8,9 product sampling analysis be the results are shown in Table 6:
Table 6: embodiment 3 products obtained therefrom composition analysis tables
Other foreign matter contents are in lot number 7～9 products: Fe≤0.0002%, Cu≤0.000001%, Ni≤0.000003%, Pb≤0.00005, Cl≤0.0005%, K
2CO
3≤ 0.03%. product appearance is colourless transparent liquid.
Above-mentioned detected result explanation, the prepared used in electronic industry potassium silicate solution of present embodiment is qualified.
Embodiment 4
Be example to produce 750kg used in electronic industry potassium silicate solution, do 3 groups of parallel tests simultaneously, its product is designated as lot number 10, lot number 11, lot number 12.Preparation process (1)～(3) are with embodiment 2;
(4) get the potassium silicate solution that makes in the step (3) and detect, detected result sees Table 7:
Table 7: embodiment 4 first potassium silicate solution composition analysis tables
According to above-mentioned analysis, lot number 11,12 product moduluses are qualified, add the 290.48kg electron-grade water, and restir 20 minutes namely obtains the used in electronic industry potassium silicate solution;
(5) lot number 10 product moduluses are defective, as calculated, add 2.24kg high pure and ultra-fine silicon powder, are heated to 95～100 ℃, insulated and stirred reaction 30 minutes, and sampling inspection results is as follows:
Lot number: 10, SiO
2: 31.62%, K
2O:14.58%, concentration of potassium silicate (K
2OnSiO
2): 46.20%, n=3.40;
Modulus is qualified, adds the 300.14kg electron-grade water, and restir 20 minutes namely obtains the used in electronic industry potassium silicate solution.Lot number 10,11,12 product sampling analysis be the results are shown in Table 8:
Table 8: embodiment 4 products obtained therefrom composition analysis tables
Other foreign matter contents are in lot number 10～12 products: Fe≤0.0002%, Cu≤0.000001%, Ni≤0.000003%, Pb≤0.00005, Cl≤0.0005%, K
2CO
3≤ 0.03%.Product appearance is colourless transparent liquid.
Above-mentioned detected result explanation, the prepared used in electronic industry potassium silicate solution of present embodiment is qualified.
Used high pure and ultra-fine silicon powder is with high-purity white carbon black (SiO among the present invention
2〉=99.98%, particle diameter is 0.5～5 micron or thinner) or high silica flour (Si 〉=99.999%, particle diameter≤5 micron) replace, also be feasible.
Claims (1)
1. the production method of a used in electronic industry potassium silicate solution, the massfraction that requires its product mesosilicic acid potassium is 28% ± 0.5%, the ratio of silicon-dioxide and the amount of substance of potassium oxide in the potassium silicate, be that modulus n is 3.40 ± 0.03, it is characterized in that: be to be that raw material reaction makes with high pure and ultra-fine silicon powder and potassium hydroxide solution, comprise the steps:
(1) according to the total mass of the potassium silicate solution of required production, calculate the quality of required high pure and ultra-fine silicon powder and potassium hydroxide solution, basis:
NSiO
2+ 2KOH=K
2OnSiO
2+ H
2O, wherein n=3.40;
According to calculation result, accurately take by weighing required high pure and ultra-fine silicon powder and potassium hydroxide solution; SiO in the described high pure and ultra-fine silicon powder
2〉=99.98%, Fe≤2ppm, particle diameter are 0.5～5 micron; Described potassium hydroxide solution is that the massfraction of ionic membrane method production is 48% potassium hydroxide solution;
(2) potassium hydroxide solution that weighs up being added doing in the reactor of lining with polytetrafluoroethylmaterial material of band stirring, heating and temperature control unit, open whipping appts, is 20%～25% with an amount of electron-grade water dilute hydrogen potassium oxide solution to its massfraction;
(3) open heating, whipping appts, make reactor temperature reach 80 ℃, insulation slowly adds the high pure and ultra-fine silicon powder, behind reinforced the finishing, continues to heat up, and reaches 95～100 ℃, insulation reaction 1 hour to reactor temperature;
(4) sampling detects, modulus n according to the cubage potassium silicate solution of dioxide-containing silica and potassium oxide, if n=3.40 ± 0.03, then the product modulus is qualified, massfraction according to potassium silicate, adding an amount of electron-grade water, to be diluted to product mesosilicic acid potassium massfraction be 28%, stirred 20 minutes, namely; If following step (5) is carried out in n＞3.43; If following step (6) is carried out in n＜3.37;
(5) if the required quality of adding potassium hydroxide solution according to the n value, is calculated in n＞3.43, add required potassium hydroxide solution and stirred 20 minutes, sampling detects, repeating step (4);
(6) if the required quality of adding the high pure and ultra-fine silicon powder according to the n value, is calculated in n＜3.37, under agitation add the high pure and ultra-fine silicon powder and be warming up to 95～100 ℃, insulation reaction 30 minutes, sampling detects, repeating step (4).
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104004393A (en) * | 2014-03-18 | 2014-08-27 | 重庆艾普化工有限公司 | Water-based inorganic zinc-rich anticorrosive paint and preparing method of high-modulus potassium silicate solution |
| CN110357672A (en) * | 2018-08-08 | 2019-10-22 | 友达晶材股份有限公司 | Aqueous silicate solution, fertilizer and preparation method and for make aqueous silicate solution or fertilizer through carbonized powder |
| CN110862283A (en) * | 2018-08-08 | 2020-03-06 | 友达晶材股份有限公司 | Fertilizer and method for producing fertilizer containing silicate aqueous solution |
| CN111099599A (en) * | 2020-01-20 | 2020-05-05 | 西安通鑫半导体辅料有限公司 | Lithium silicate solution and preparation method thereof |
| CN111204772A (en) * | 2020-01-20 | 2020-05-29 | 西安通鑫半导体辅料有限公司 | High-purity high-modulus potassium silicate solution and preparation method thereof |
| CN112624133A (en) * | 2020-12-22 | 2021-04-09 | 杭州威斯诺威科技有限公司 | Preparation method of environment-friendly potassium silicate solution |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104004393A (en) * | 2014-03-18 | 2014-08-27 | 重庆艾普化工有限公司 | Water-based inorganic zinc-rich anticorrosive paint and preparing method of high-modulus potassium silicate solution |
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| CN110862283A (en) * | 2018-08-08 | 2020-03-06 | 友达晶材股份有限公司 | Fertilizer and method for producing fertilizer containing silicate aqueous solution |
| CN111099599A (en) * | 2020-01-20 | 2020-05-05 | 西安通鑫半导体辅料有限公司 | Lithium silicate solution and preparation method thereof |
| CN111204772A (en) * | 2020-01-20 | 2020-05-29 | 西安通鑫半导体辅料有限公司 | High-purity high-modulus potassium silicate solution and preparation method thereof |
| CN112624133A (en) * | 2020-12-22 | 2021-04-09 | 杭州威斯诺威科技有限公司 | Preparation method of environment-friendly potassium silicate solution |
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Application publication date: 20130828 |