CN105776877A - Method for preparing glass fiber from waste of phosphoric acid production - Google Patents
Method for preparing glass fiber from waste of phosphoric acid production Download PDFInfo
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- CN105776877A CN105776877A CN201610061936.4A CN201610061936A CN105776877A CN 105776877 A CN105776877 A CN 105776877A CN 201610061936 A CN201610061936 A CN 201610061936A CN 105776877 A CN105776877 A CN 105776877A
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- glass fibre
- fluorine
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C13/00—Fibre or filament compositions
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/20—Halides
- C01F11/22—Fluorides
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- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention discloses a method for preparing a glass fiber from waste of phosphoric acid production. The method includes the steps of absorbing fluorine-containing gas produced in phosphoric acid production with water to prepare fluorosilicic acid; carrying out press filtration separation on slurry obtained after neutralizing the fluorosilicic acid with lime milk, drying a filter cake until the moisture content is less than or equal to 1%, and crushing the filter cake to the particle size required by glass fiber powder feeding, to obtain a fluorine-containing material; and preparing a glass fiber mixed material from the obtained fluorine-containing material, and producing the glass fiber, wherein the glass fiber mixed material comprises the following components by weight: 160-210 parts of quick lime, 140-190 parts of pyrophyllite A, 110-160 parts of pyrophyllite B, 45-75 parts of dolomite, 45-75 parts of colemanite, 200-250 parts of white afrodite, 40-60 parts of kaolin A, 30-50 parts of kaolin B, 28-38 parts of spodumene, 11-15 parts of albite, 22-28 parts of the fluorine-containing material, and 3-6 parts of a composite clarificant.
Description
Technical field
The present invention relates to the production method of glass fibre, the Litter particularly relating to phosphoric acid production prepares the method for glass fibre.
Background technology
Rock phosphate in powder accompaniment and fluorite are the main sources of fluorine resource.Along with non-renewable fluorite resource amount reduces year by year, the substitute products of fluorite are increasingly paid close attention to by industry.Whole world fluorite reserves are about 600,000,000 tons, calculate by 50% Oil repellent, and fluorine total amount also only has about 300,000,000 tons.And the rock phosphate in powder reserves about 60,000,000,000 tons that the world is known, the Oil repellent in rock phosphate in powder is 2%～4%, and corresponding fluorine total amount is 1,200,000,000 ~ 2,400,000,000 tons.The fluorine resource of association in rock phosphate in powder is big more than the reserves of fluorite.
Rock phosphate in powder is the primary raw material of Wet-process Phosphoric Acid Production, can produce substantial amounts of fluoro-gas in production process of phosphoric acid, if entering air, human body and natural environment will be produced high risks.It is usually silicon tetrafluoride gas, absorbs with water and generate hexafluosilicic acid, then process again.Produced tail gas in Wet-process Phosphoric Acid Production, after water absorbs, obtained liquid is hexafluosilicic acid.Mean fluorine silicic acid concentration 1-2%, ton phosphate produces hexafluosilicic acid 0.4m3, its main component is the hexafluosilicic acid of low concentration, silica gel and minimal amount of phosphoric acid.Process to by-product fluosilicic acid, phosphoric acid by wet process industry is typically all discharge after employing neutralizes, and liquid phase returns the pattern doing process water.In addition with few part wet phosphoric acid producer, producing calcium fluoride, cryolite, prodan, sodium fluoride and Fluohydric acid. etc. with hexafluosilicic acid, but it is limited to there is market capacity, the technological process of production is long, the shortcomings such as production cost is high, bring relatively hang-up to the comprehensive utilization of hexafluosilicic acid.Although the production technological process of prodan is the shortest, production cost is minimum, but market capacity is extremely limited, and the concentration of its hexafluosilicic acid is generally individually at 10-12%, additionally needs the waste water of its generation is neutralized process.The production of above fluoride, was not suitable for phosphoric acid by wet process enterprise when present stage.Therefore overwhelming majority producer is all the mode stacked after adopting simple neutralisation treatment, this brings lasting fluoride pollution to surrounding enviroment, is unfavorable for the long term growth of phosphoric acid by wet process industry.
Summary of the invention
For above-mentioned deficiency of the prior art, the Litter utilizing phosphoric acid production provided by the invention prepares the method for glass fibre can substitute, by calcium fluoride prepared by the waste gas produced in recovery production process of phosphoric acid, the fluorite produced in glass fibre raw material completely.
In order to reach foregoing invention purpose, the technical solution used in the present invention is:
A kind of method that Litter utilizing phosphoric acid production prepares glass fibre is provided, comprising:
Absorb a large amount of fluoro-gas produced in production process of phosphoric acid with water, prepare into hexafluosilicic acid；Adopting lime cream that the hexafluosilicic acid obtained is neutralized process, the slurry filter pressing after neutralizing separated afterwards, filter cake is dried to moisture content less than or equal to 1%, is crushed to the glass fibre required granularity that feeds intake and obtains fluorine-containing material；The fluorine-containing material of gained is used for preparing glass fibre batch and carries out the production of glass fibre；
Described glass fibre batch includes the component that following weight proportion is following:
Quick lime 160 ~ 210 parts；Pyrophillite A140 ~ 190 part；Pyrophillite B110 ~ 160 part；Dolomite 45 ~ 75 parts；Colemanite 45～75 parts；White afrodite 200～250 parts；Kaolin A40～60 part；Kaolin B30～50 part；Spodumene 28～38 parts；Albite 11～15 parts；Fluorine-containing material 22～28 parts；Compound clarifier 3～6 parts；In glass fibre batch, each component proportion sum is 1000 parts；
Wherein, fluorine-containing material is mainly made up of the component of following weight portion: 60～70 parts of calcium fluoride, silica 15 ~ 25 parts.
The invention have the benefit that the present invention adopts fluorine-containing material substitution fluorite to produce glass fibre, reduce produced tail gas environmental pollution in phosphoric acid production not only by comprehensive utilization, turned waste into wealth；And the glass fibre indices that produces all can be up to standard, its precursor LOI can reach about 0.5%, dry yarn moisture about 10%, intensity can reach more than 0.35.
Detailed description of the invention
Below the specific embodiment of the present invention is described; so that those skilled in the art understand the present invention; it is to be understood that; the invention is not restricted to the scope of detailed description of the invention; to those skilled in the art; as long as various changes limit and in the spirit and scope of the present invention determined, these changes are apparent from, and all utilize the innovation and creation of present inventive concept all at the row of protection in appended claim.
This utilizes the method that the Litter of phosphoric acid production prepares glass fibre to include:
Absorb a large amount of fluoro-gas produced in production process of phosphoric acid with water, prepare into hexafluosilicic acid；Adopting lime cream that the hexafluosilicic acid obtained is neutralized process, the slurry filter pressing after neutralizing separated afterwards, filter cake is dried to moisture content less than or equal to 1%, is crushed to the glass fibre required granularity that feeds intake and obtains fluorine-containing material；The fluorine-containing material of gained is used for preparing glass fibre batch and carries out the production of glass fibre；
Described glass fibre batch includes the component of following weight portion:
Quick lime 160 ~ 210 parts；Pyrophillite A140 ~ 190 part；Pyrophillite B110 ~ 160 part；Dolomite 45 ~ 75 parts；Colemanite 45～75 parts；White afrodite 200～250 parts；Kaolin A40～60 part；Kaolin B30～50 part；Spodumene 28～38 parts；Albite 11～15 parts；Fluorine-containing material 22～28 parts；Compound clarifier 3～6 parts；In glass fibre batch, each component proportion sum is 1000 parts；
Wherein, fluorine-containing material is mainly made up of the component of following weight portion: 60～70 parts of calcium fluoride, silica 15 ~ 25 parts；Above-mentioned pyrophillite A and pyrophillite B comes from the different places of production, Kaolin A and Kaolin B respectively and comes from the different places of production respectively.
In one embodiment of the invention, the calcium fluoride of gained is used for preparing glass fibre batch carry out the production of glass fibre and farther include:
According to the formula proportion of described glass fibre batch, take each material, pulverize, remix uniformly；Found at 1500 DEG C ~ 1600 DEG C, operation access is entered after being then passed through clarification, homogenizing, flow out in the platinum bushing plate in 800～5000 holes, the temperature flowed out from platinum bushing plate controls at 1280 DEG C～1320 DEG C, then after one layer of macromolecule emulsion of its surface-coated, it is wrapped on headstock wire drawing, prepares.
Wherein, macromolecule emulsion is binding agent, becomes cured dose, lubricant or antistatic additive；Binding agent therein can be phenolic aldehyde-neoprene, organic silica gel or polyvinyl acetate, and lubricant can be silicone oil, fatty acid amide, oleic acid, polyester, synthetic ester or carboxylic acid；Antistatic additive can be ethoxylated fat race alkylamine；Described calcium fluoride, dolomite, albite, compound clarifier and calcium lime powder were broken to 100 mesh sieves, and colemanite was crushed to 200 mesh sieves, and white afrodite, pyrophillite A, pyrophillite B, Kaolin A, Kaolin B and spodumene were crushed to 325 mesh sieves.
Embodiment 1
Produce 100kg glass fibre, weigh the raw material of following weight:
Quick lime 16kg；Pyrophillite A17kg；Pyrophillite B13.5kg；
Dolomite 7.3kg；Colemanite 6kg；White afrodite 23.4kg；
Kaolin A5kg；Kaolin B4.1kg；Spodumene 3.4kg
Albite 1.1kg；Fluorine-containing material 2.8kg；Compound clarifier 0.4kg；
Wherein, fluorine-containing material is mainly made up of the component of following weight portion: 61 parts of calcium fluoride, silicon dioxide 24 parts；
The composition of pyrophillite (A, B): SiO2>=74%, Al2O3>=15.0%, Fe2O3≤ 0.55%, H2O≤1%；Pyrophillite A and pyrophillite B comes from the different places of production respectively；The composition of dolomite: CaO >=30%, Fe2O3≤ 0.2%, MgO >=19.5%, H2O≤1%；The composition of colemanite: CaO >=27%, Fe2O3≤ 0.10%, SiO2≤ 6.5%, B2O3>=39%, H2O≤1%；The composition of quick lime: CaO >=85%, Fe2O3≤ 0.25%, MgO≤3%, H2O≤1%。
The composition of white afrodite: SiO2>=81%, Al2O3>=10%, Fe2O3≤ 0.60%, H2O≤1%；The composition of Kaolin (A, B): SiO2>=40%, Al2O3>=36%, Fe2O3≤ 0.9%, H2O≤1%；Kaolin A and Kaolin B comes from the different places of production respectively；The composition of spodumene: SiO2>=56%, Al2O3>=19%, Fe2O3≤ 0.9%, H2O≤1%；The composition of albite: SiO2>=70%, Al2O3>=16%, Fe2O3≤ 0.65%, Na2O+K2O >=7.5%, H2O≤1%；
The composition of fluorine-containing material: CaF2=61%, SiO2=24%, H2O=1%, surplus is impurity；The composition of compound clarifier: SO3>=21%, H2O≤1%；Above-mentioned percentage ratio is mass ratio.
The preparation method of fluorine-containing material is: absorbs a large amount of fluoro-gas produced in production process of phosphoric acid with water, prepares into hexafluosilicic acid；Adopting lime cream that the hexafluosilicic acid obtained is neutralized process, the slurry filter pressing after neutralizing separated afterwards, filter cake is dried to moisture content less than or equal to 1%, is crushed to the glass fibre required granularity that feeds intake and obtains fluorine-containing material.
The preparation method of glass fibre is: according to the proportioning mix homogeneously raw material of component each in glass fibre batch；Found at 1500 DEG C ~ 1600 DEG C, entering operation access after being then passed through clarification, homogenizing, flow out in the platinum bushing plate in 800～5000 holes, the temperature flowed out from platinum bushing plate controls at 1280 DEG C～1320 DEG C, then, after one layer of macromolecule emulsion of its surface-coated, it is wrapped on headstock wire drawing.Wherein, macromolecule emulsion is coupling agent, binding agent, cured dose of one-tenth, lubricant and/or antistatic additive；Calcium fluoride, dolomite, albite, compound clarifier and quick lime cross 100 mesh sieves before founding, and colemanite crosses 200 mesh sieves, and white afrodite, pyrophillite A, pyrophillite B, Kaolin A, Kaolin B and spodumene cross 325 mesh sieves.
Each index of the glass fibre that the formula according to the present embodiment offer produces is as follows:
Precursor count is 2400, precursor LOI is 0.5%, dry yarn moisture is 10%；Penetration period 15s, intensity 0.45MPa.
Embodiment 2
Produce 100kg glass fibre, weigh the raw material of following weight:
Quick lime 18.8kg；Pyrophillite A15.8kg；Pyrophillite B15.83kg；
Dolomite 5kg；Colemanite 7.4kg；White afrodite 20.5kg；
Kaolin A4.2kg；Kaolin B5kg；Spodumene 2.9kg
Albite 1.5kg；Fluorine-containing material 2.5kg；Compound clarifier 0.57kg；
Wherein, fluorine-containing material is mainly made up of the component of following weight portion: 66 parts of calcium fluoride, silica 19 parts；The composition of fluorine-containing material: CaF2=66%, SiO2=19%, H2O=0.8%, surplus is impurity；Contained by other raw materials in the present embodiment, the ratio of chemical composition and each chemical composition, the preparation method of fluorine-containing material and the preparation method of glass fibre are consistent with embodiment 1, just repeat no more herein.
Each index of the glass fibre that the formula according to the present embodiment offer produces is as follows:
Precursor count is 400, precursor LOI is 0.45%, dry yarn moisture is 9%；Penetration period 20s, stiffness 110mm.
Embodiment 3
Produce 100kg glass fibre, weigh the raw material of following weight
Quick lime 20.kg；Pyrophillite A18.0kg；Pyrophillite B11.1kg；
Dolomite 6kg；Colemanite 4.5kg；White afrodite 24.2kg；
Kaolin A5.8kg；Kaolin B3.1kg；Spodumene 3.5kg
Albite 1.1kg；Fluorine-containing material 2.2kg；Compound clarifier 0.5kg；
Wherein, fluorine-containing material is mainly made up of the component of following weight portion: 70 parts of calcium fluoride, silica 16 parts；The composition of fluorine-containing material: CaF2=70%, SiO2=16%, H2O=0.5%, surplus is impurity；Contained by other raw materials in the present embodiment, the ratio of chemical composition and each chemical composition, the preparation method of fluorine-containing material and the preparation method of glass fibre are consistent with embodiment 1, just repeat no more herein.
Each index of the glass fibre that the formula according to the present embodiment offer produces is as follows:
Precursor count is 500, precursor LOI is 0.3%, dry yarn moisture is 8%；Intensity 0.35MPa.
In sum, it is appreciated that by above-described embodiment and testing result, using calcium fluoride prepared by the Litter produced in production process of phosphoric acid to substitute the fluorite in glass fibre raw material completely, to carry out the production of glass fibre be feasible, adopt production method provided by the invention, it is possible not only to solve the pollution problem of calcium fluoride waste material, and use it for the raw material producing glass fibre, the quality of prepared glass fibre is better, has bigger prospect.
Claims (4)
1. the Litter utilizing phosphoric acid production prepares the method for glass fibre, it is characterised in that including:
Absorb a large amount of fluoro-gas produced in production process of phosphoric acid with water, prepare into hexafluosilicic acid；Adopting lime cream that the hexafluosilicic acid obtained is neutralized process, the slurry filter pressing after neutralizing separated afterwards, filter cake is dried to moisture content less than or equal to 1%, is crushed to the glass fibre required granularity that feeds intake and obtains fluorine-containing material；The fluorine-containing material of gained is used for preparing glass fibre batch and carries out the production of glass fibre；
Described glass fibre batch includes the component of following weight portion:
Quick lime 160 ~ 210 parts；Pyrophillite A140 ~ 190 part；Pyrophillite B110 ~ 160 part；Dolomite 45 ~ 75 parts；Colemanite 45～75 parts；White afrodite 200～250 parts；Kaolin A40～60 part；Kaolin B30～50 part；Spodumene 28～38 parts；Albite 11～15 parts；Fluorine-containing material 22～28 parts；Compound clarifier 3～6 parts；In glass fibre batch, each component proportion sum is 1000 parts；
Wherein, described fluorine-containing material is mainly made up of the component of following weight portion: 60～70 parts of calcium fluoride, silica 15 ~ 25 parts.
2. the method that the Litter utilizing phosphoric acid production according to claim 1 prepares glass fibre, it is characterised in that described the calcium fluoride of gained is used for preparing glass fibre batch carries out the production of glass fibre and farther include:
According to the formula proportion of described glass fibre batch, take each material, pulverize, remix uniformly；Found at 1500 DEG C ~ 1600 DEG C, operation access is entered after being then passed through clarification, homogenizing, flow out in the platinum bushing plate in 800～5000 holes, the temperature flowed out from platinum bushing plate controls at 1280 DEG C～1320 DEG C, then after one layer of macromolecule emulsion of its surface-coated, it is wrapped on headstock wire drawing, prepares.
3. the method that the Litter utilizing phosphoric acid production according to claim 2 prepares glass fibre, it is characterized in that, described calcium fluoride, dolomite, albite, compound clarifier and calcium lime powder were broken to 100 mesh sieves, colemanite was crushed to 200 mesh sieves, and white afrodite, pyrophillite A, pyrophillite B, Kaolin A, Kaolin B and spodumene were crushed to 325 mesh sieves.
4. the method that the Litter utilizing phosphoric acid production according to Claims 2 or 3 prepares glass fibre, it is characterised in that described macromolecule emulsion is binding agent, lubricant or antistatic additive.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610061936.4A CN105776877A (en) | 2016-01-29 | 2016-01-29 | Method for preparing glass fiber from waste of phosphoric acid production |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610061936.4A CN105776877A (en) | 2016-01-29 | 2016-01-29 | Method for preparing glass fiber from waste of phosphoric acid production |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS4939565A (en) * | 1972-08-22 | 1974-04-13 | ||
| CN102167519A (en) * | 2010-12-31 | 2011-08-31 | 巨石集团有限公司 | Method for manufacturing glass fibers by circularly using fluorine-containing waste slag |
| CN103058513A (en) * | 2013-01-05 | 2013-04-24 | 内江华原电子材料有限公司 | Compound clarifying agent, preparation method thereof and method for preparing E glass fiber by adopting compound clarifying agent |
| CN104402214A (en) * | 2014-10-31 | 2015-03-11 | 内江华原电子材料有限公司 | Method for producing glass fiber by using pulping and paper-making white mud |
| CN104944803A (en) * | 2015-06-30 | 2015-09-30 | 四川航天五源复合材料有限公司 | Basalt continuous fiber sizing agent |
-
2016
- 2016-01-29 CN CN201610061936.4A patent/CN105776877A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS4939565A (en) * | 1972-08-22 | 1974-04-13 | ||
| CN102167519A (en) * | 2010-12-31 | 2011-08-31 | 巨石集团有限公司 | Method for manufacturing glass fibers by circularly using fluorine-containing waste slag |
| CN103058513A (en) * | 2013-01-05 | 2013-04-24 | 内江华原电子材料有限公司 | Compound clarifying agent, preparation method thereof and method for preparing E glass fiber by adopting compound clarifying agent |
| CN104402214A (en) * | 2014-10-31 | 2015-03-11 | 内江华原电子材料有限公司 | Method for producing glass fiber by using pulping and paper-making white mud |
| CN104944803A (en) * | 2015-06-30 | 2015-09-30 | 四川航天五源复合材料有限公司 | Basalt continuous fiber sizing agent |
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Application publication date: 20160720 |