CN107777690A - A kind of method for purifying silicon source - Google Patents

A kind of method for purifying silicon source Download PDF

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Publication number
CN107777690A
CN107777690A CN201610734405.7A CN201610734405A CN107777690A CN 107777690 A CN107777690 A CN 107777690A CN 201610734405 A CN201610734405 A CN 201610734405A CN 107777690 A CN107777690 A CN 107777690A
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Prior art keywords
acid
silicon source
purity
industrial
kiselgel
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CN201610734405.7A
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Chinese (zh)
Inventor
肖启发
李泽工
阎云朝
邓林
候强
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Sichuan Xilong Chemical Co Ltd
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Sichuan Xilong Chemical Co Ltd
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Priority to CN201610734405.7A priority Critical patent/CN107777690A/en
Publication of CN107777690A publication Critical patent/CN107777690A/en
Pending legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/113—Silicon oxides; Hydrates thereof
    • C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/08—Compounds containing halogen
    • C01B33/10—Compounds containing silicon, fluorine, and other elements
    • C01B33/103—Fluosilicic acid; Salts thereof
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/113—Silicon oxides; Hydrates thereof
    • C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/20—Silicates
    • C01B33/32—Alkali metal silicates
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/80—Compositional purity

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Silicon Compounds (AREA)
  • Cosmetics (AREA)

Abstract

This patent is related to a kind of method of industrial Kiselgel A purifying, specially a kind of method for purifying silicon source.Industrial Kiselgel A is soaked using high-purity watery hydrochloric acid, metal ion in silica gel is dissolved and leached, with pure water washing by soaking, the silicon source of high-purity is obtained after drying, the industrial more micropores of Kiselgel A and, 650 800 ㎡s/g bigger than surface, if being converted into particle size, equivalent to fineness more than 5,000,000 mesh, this is the fineness that mechanical crushing can not be reached.Single metal ion in product of the present invention is below 1ppm, and total metal content is less than 10ppm；Fluosilicic acid is neutralized and can be made into various high-purity fluosilicates；Highly pure active silica gel after drying directly reacts to obtain sodium silicate nanahydrate with sodium hydroxide solution.

Description

A kind of method for purifying silicon source
Technical field
This patent is related to a kind of method of industrial Kiselgel A purifying, specially a kind of method for purifying silicon source.
Background technology：
Silicic acid, fluosilicic acid and its esters in reagent industry, the silicon source majority used is glass sand, due to using mechanical powder Broken, its fineness is restricted, and the purity of quartz sand is relatively low, so as to limit silicic acid, sodium metasilicate, fluosilicic acid and its esters purity Improve.On the other hand, active relatively low due to quartz sand when producing fluosilicic acid and its esters, producing will during fluosilicic acid The reaction temperature asked is higher, causes a large amount of of ocratation to escape, environmental pollution is extremely serious.
The mode of purifying silicon is very ripe in electronics industry, can pass through chlorine silicon compound gas using quartz sand as raw material Change is purified, reduced, taking out the processes such as monocrystalline and obtain the extra high monocrystalline silicon of purity, for electronics industry.Using this method purifying silicon, Its complex process, investment is high, production cost is high, environmental pollution is serious.
Industrial Kiselgel A is than surface 650-800 ㎡/g, if being converted into particle size, equivalent to more than 5,000,000 mesh thin Degree, this is the fineness that mechanical crushing can not be reached.
The content of the invention
The present invention is directed to problem of the prior art, there is provided a kind of method for purifying silicon source, it is inexpensive using source very abundant Industrial silicone be raw material, through pickling, washing obtain highly pure active silica gel, highly pure active silica gel is directly dried, dried, is obtained High-purity silicic acid.
A kind of method for purifying silicon source, it is characterised in that comprise the following steps：
A, industrial Kiselgel A is soaked using high-purity watery hydrochloric acid, the metal ion in silica gel is dissolved and leached, utilized The industrial more micropores of Kiselgel A and, 650-800 ㎡/g bigger than surface, if being converted into particle size, more than 5,000,000 mesh Fineness, this is the fineness that mechanical crushing can not be reached；
B, with pure water washing by soaking；
C, the silicon source of high-purity is obtained after drying
Silicon source product for silicic acid, sodium silicate nanahydrate, fluosilicic acid, fluosilicate.
Preparation principle：Silica gel micropore is passed through with watery hydrochloric acid, dissolved metal salt, metal ion is removed with pure water, obtains Highly pure active silica gel, silicic acid, sodium silicate nanahydrate, fluosilicic acid and its esters is then made.
SiO2·nH2O+NaOH→Na2SiO3+H2O
SiO2·nH2O+HF→H2SiF6+H2O
H2SiF6+Na2CO3→Na2SiF6↓+H2O+CO2↑
H2SiF6+KOH→K2SiF6↓+H2O
1. silicic acid
1.1 in 1000L Plastic Drums, add technical grade silica gel 200Kg, add pure water to cover material.
1.2 place 1h, treat that material reaction finishes, stir evenly.
1.3 discharge solution, with pure water rinse 2-3 time it is limpid to solution, add pure water cover material, addition hydrochloric acid 10L, stir It is even.Stand overnight.
1.4 discharge solution, are rinsed to washing lotion PH6-7, by silicic acid in being dehydrated on centrifuge repeatedly with pure water.
The wet feed that centrifuge comes out is put into drying room and dried by 1.5.
1.6 are put into two layers of polybag, labeling.
1.7 notice Quality Control Department the full review of sampling.
After 1.8 full inspections are qualified, check weight and tighten packing inside bag, be put on its surface and fill in content《The quality certification》, Outer packaging bag is tightened, silicic acid enters warehouse for finished product
2. sodium silicate nanahydrate
2.1 add the silicic acid of drying in 1000L stainless steel cauldrons, add 500 kilograms of pure water, add solid sodium hydroxide 300 Kilogram, lead to steam-stirring dissolving, stand overnight
2.2 strain clear liquid in crystallizer, add solid sodium hydroxide 120 kg, keep solution about 1000L, after solution is slightly cold, Add a small amount of sodium silicate nanahydrate crystal seed, crystallisation by cooling.
2.3 by crystalline solid in being dehydrated on centrifuge, washed with a small amount of ethanol.Mother liquor and get rid of liquid and apply mechanically.
The 2.4 wet feed airings for coming out centrifuge.
2.5 are put into two layers of polybag, labeling.
2.6 notice Quality Control Department the full review of sampling.
After 2.7 full inspections are qualified, check weight and tighten packing inside bag, be put on its surface and fill in content《The quality certification》, Outer packaging bag is tightened, sodium silicate nanahydrate enters warehouse for finished product
3. fluosilicic acid
3.1 take silica gel 300Kg, are boiled three times with 10% hydrochloric acid, and acid solution is changed into yellowish from dark red, are washed with water to PH4.0, dry and add Water immersion, dry, quadruplication, obtain silicic acid.
In 800L Plastic Drum Nei Jiajia water 260Kg, take silicic acid 316Kg, 55% hydrofluoric acid 560Kg；Hydrofluoric acid adds in three times Enter, additional cooling water, control reaction is gentle.Temperature is no more than 500C is advisable, it is advisable with not producing acid mist, is stood overnight.
3.2 filter fluosilicic acid in 50L plastics filter pocket, and filtrate is collected in 200L turnover barrels.
3.3 hand over inspection；Remaining silicic acid uses as synthesis next time.
3.4 after the assay was approved, and packaging is sent with return on qualification list and batch number.
3.5 electron level fluosilicic acid enter warehouse for finished product
4. potassium fluosilicate
4.1 add water 170Kg, silicic acid 200Kg in 800L Plastic Drums, according to reaction severe degree（Temperature is less than 500C, with not Producing acid mist is advisable）, fraction（3-4 times）Add hydrofluoric acid（55%）About 370Kg, acid adding process stirring, stands overnight.
4.2 take out the silicate fluoride solution of clarification and are filtered with 50L plastics filter pocket, and filtrate is collected in 200L turnover barrels, taken 180Kg fluosilicic acid is synthesized in bucket in 800L plastics, is diluted with pure water 60Kg.It is standby for synthesizing potassium fluosilicate.
4.3 in stainless-steel pan, adds 380L pure water and is heated to 400C or so, potassium carbonate is added under agitation 65kg, appropriate silicate fluoride solution is added after dissolving, filtered after placing about 8h.Filtrate is standby for synthesizing potassium fluosilicate.
4.4 have in the Plastic Drum of 7.3 fluosilicic acid in 800L storages, under agitation, are slowly added into 7.4 solution of potassium carbonate （Feed time 3-4h）, 400L or so is about added, PH2.8-3.0 is now required, stands overnight.
4.5 filter potassium fluosilicate with two layers of cloth, and potassium fluosilicate is dehydrated in drier.Potassium fluosilicate filtrate can be used for dilute Release fluosilicic acid or solution of potassium carbonate.
4.6 by the potassium fluosilicate after dehydration in drying room 80-900It is qualified that content is dried in C, crushes, pack, labeling.
4.7 notice Quality Control Department the full review of sampling.
4.8 after the assay was approved, and packaging is sent with return on qualification list and batch number.
4.9 potassium fluosilicates enter warehouse for finished product
5. prodan
5.1 add water 170Kg, silicic acid 200Kg in 800L Plastic Drums, according to reaction severe degree（Temperature is less than 500C, with not Producing acid mist is advisable）, fraction（3-4 times）Add hydrofluoric acid（55%）About 370Kg, acid adding process stirring, stands overnight.
5.2 take out the silicate fluoride solution of clarification and are filtered with 50L plastics filter pocket, and filtrate is collected in 200L turnover barrels, taken 180Kg fluosilicic acid is synthesized in bucket in 800L plastics, is diluted with pure water 60Kg.It is standby for synthesizing potassium fluosilicate.
5.3 in stainless-steel pan, adds 250L pure water and is heated to 700C or so, soda ash 90kg is added under agitation, Appropriate silicate fluoride solution is added after dissolving, is filtered after placing about 8h, filtrate is diluted to 400L or so with pure water.Filtrate is used for It is standby to synthesize prodan.
5.4 are warming up to 70 in 800L Plastic Drum addition 350L silicate fluoride solutions, logical steam0C or so, in stirring condition Under, sodium carbonate liquor is slowly added into, 350L or so is about added, now requires PH2.5-3.0, stand overnight.
5.5 filter prodan with two layers of cloth, and prodan is dehydrated in drier.Prodan filtrate can be used for dilute Release fluosilicic acid or sodium carbonate liquor.
5.6 by the prodan after dehydration in drying room 80-900It is qualified that content is dried in C, crushes, pack, labeling.
5.7 notice Quality Control Department the full review of sampling.
5.8 after the assay was approved, and packaging is sent with return on qualification list and batch number.
5.9 prodans enter warehouse for finished product
This technology uses the inexpensive industrial silicone of source very abundant as raw material, and highly pure active silica gel is obtained through pickling, washing, will Highly pure active silica gel is directly dried, dried, and obtains high-purity silicic acid.Highly pure active silica gel after drying directly reacts with hydrofluoric acid To high pure electronic grade fluosilicic acid, the single metal ion in its product is below 1ppm, and total metal content is less than 10ppm；By fluorine silicon Acid neutralizes and can be made into various high-purity fluosilicates；Highly pure active silica gel after drying directly reacts to obtain nine with sodium hydroxide solution Hydrated sodium silicate.
Embodiment
This patent is described further with reference to embodiment.
1. silicic acid
1.1 in 1000L Plastic Drums, add technical grade silica gel 200Kg, add pure water to cover material.
1.2 place 1h, treat that material reaction finishes, stir evenly.
1.3 discharge solution, with pure water rinse 2-3 time it is limpid to solution, add pure water cover material, addition hydrochloric acid 10L, stir It is even.Stand overnight.
1.4 discharge solution, are rinsed to washing lotion PH6-7, by silicic acid in being dehydrated on centrifuge repeatedly with pure water.
The wet feed that centrifuge comes out is put into drying room and dried by 1.5.
1.6 are put into two layers of polybag, labeling.
1.7 notice Quality Control Department the full review of sampling.
After 1.8 full inspections are qualified, check weight and tighten packing inside bag, be put on its surface and fill in content《The quality certification》, Outer packaging bag is tightened, silicic acid enters warehouse for finished product
2. sodium silicate nanahydrate
2.1 add the silicic acid of drying in 1000L stainless steel cauldrons, add 500 kilograms of pure water, add solid sodium hydroxide 300 Kilogram, lead to steam-stirring dissolving, stand overnight
2.2 strain clear liquid in crystallizer, add solid sodium hydroxide 120 kg, keep solution about 1000L, after solution is slightly cold, Add a small amount of sodium silicate nanahydrate crystal seed, crystallisation by cooling.
2.3 by crystalline solid in being dehydrated on centrifuge, washed with a small amount of ethanol.Mother liquor and get rid of liquid and apply mechanically.
The 2.4 wet feed airings for coming out centrifuge.
2.5 are put into two layers of polybag, labeling.
2.6 notice Quality Control Department the full review of sampling.
After 2.7 full inspections are qualified, check weight and tighten packing inside bag, be put on its surface and fill in content《The quality certification》, Outer packaging bag is tightened, sodium silicate nanahydrate enters warehouse for finished product
3. fluosilicic acid
3.1 take silica gel 300Kg, are boiled three times with 10% hydrochloric acid, and acid solution is changed into yellowish from dark red, are washed with water to PH4.0, dry and add Water immersion, dry, quadruplication, obtain silicic acid.
In 800L Plastic Drum Nei Jiajia water 260Kg, take silicic acid 316Kg, 55% hydrofluoric acid 560Kg；Hydrofluoric acid adds in three times Enter, additional cooling water, control reaction is gentle.Temperature is no more than 500C is advisable, it is advisable with not producing acid mist, is stood overnight.
3.2 filter fluosilicic acid in 50L plastics filter pocket, and filtrate is collected in 200L turnover barrels.
3.3 hand over inspection；Remaining silicic acid uses as synthesis next time.
3.4 after the assay was approved, and packaging is sent with return on qualification list and batch number.
3.5 electron level fluosilicic acid enter warehouse for finished product
6. potassium fluosilicate
4.1 add water 170Kg, silicic acid 200Kg in 800L Plastic Drums, according to reaction severe degree（Temperature is less than 500C, with not Producing acid mist is advisable）, fraction（3-4 times）Add hydrofluoric acid（55%）About 370Kg, acid adding process stirring, stands overnight.
4.2 take out the silicate fluoride solution of clarification and are filtered with 50L plastics filter pocket, and filtrate is collected in 200L turnover barrels, taken 180Kg fluosilicic acid is synthesized in bucket in 800L plastics, is diluted with pure water 60Kg.It is standby for synthesizing potassium fluosilicate.
4.3 in stainless-steel pan, adds 380L pure water and is heated to 400C or so, potassium carbonate is added under agitation 65kg, appropriate silicate fluoride solution is added after dissolving, filtered after placing about 8h.Filtrate is standby for synthesizing potassium fluosilicate.
4.4 have in the Plastic Drum of 7.3 fluosilicic acid in 800L storages, under agitation, are slowly added into 7.4 solution of potassium carbonate （Feed time 3-4h）, 400L or so is about added, PH2.8-3.0 is now required, stands overnight.
4.5 filter potassium fluosilicate with two layers of cloth, and potassium fluosilicate is dehydrated in drier.Potassium fluosilicate filtrate can be used for dilute Release fluosilicic acid or solution of potassium carbonate.
4.6 by the potassium fluosilicate after dehydration in drying room 80-900It is qualified that content is dried in C, crushes, pack, labeling.
4.7 notice Quality Control Department the full review of sampling.
4.8 after the assay was approved, and packaging is sent with return on qualification list and batch number.
4.9 potassium fluosilicate enters warehouse for finished product
7. prodan
5.1 add water 170Kg, silicic acid 200Kg in 800L Plastic Drums, according to reaction severe degree（Temperature is less than 500C, with not Producing acid mist is advisable）, fraction（3-4 times）Add hydrofluoric acid（55%）About 370Kg, acid adding process stirring, stands overnight.
5.2 take out the silicate fluoride solution of clarification and are filtered with 50L plastics filter pocket, and filtrate is collected in 200L turnover barrels, taken 180Kg fluosilicic acid is synthesized in bucket in 800L plastics, is diluted with pure water 60Kg.It is standby for synthesizing potassium fluosilicate.
5.3 in stainless-steel pan, adds 250L pure water and is heated to 700C or so, soda ash 90kg is added under agitation, Appropriate silicate fluoride solution is added after dissolving, is filtered after placing about 8h, filtrate is diluted to 400L or so with pure water.Filtrate is used for It is standby to synthesize prodan.
5.4 are warming up to 70 in 800L Plastic Drum addition 350L silicate fluoride solutions, logical steam0C or so, in stirring condition Under, sodium carbonate liquor is slowly added into, 350L or so is about added, now requires PH2.5-3.0, stand overnight.
5.5 filter prodan with two layers of cloth, and prodan is dehydrated in drier.Prodan filtrate can be used for dilute Release fluosilicic acid or sodium carbonate liquor.
5.6 by the prodan after dehydration in drying room 80-900It is qualified that content is dried in C, crushes, pack, labeling.
5.7 notice Quality Control Department the full review of sampling.
5.8 after the assay was approved, and packaging is sent with return on qualification list and batch number.
5.9 prodans enter warehouse for finished product.

Claims (2)

  1. A kind of 1. method for purifying silicon source, it is characterised in that comprise the following steps：
    A, industrial Kiselgel A is soaked using high-purity watery hydrochloric acid, the metal ion in silica gel is dissolved and leached, utilized The industrial more micropores of Kiselgel A and, 650-800 ㎡/g bigger than surface, if being converted into particle size, more than 5,000,000 mesh Fineness；
    B, with pure water washing by soaking；
    C, the silicon source of high-purity is obtained after drying.
  2. A kind of 2. method for purifying silicon source according to claim 1, it is characterised in that：The silicon source product chatted be silicic acid, Sodium silicate nanahydrate, fluosilicic acid, fluosilicate.
CN201610734405.7A 2016-08-28 2016-08-28 A kind of method for purifying silicon source Pending CN107777690A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1997622A1 (en) * 2007-05-25 2008-12-03 AGC Flat Glass Europe SA Fireproof glazing

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1997622A1 (en) * 2007-05-25 2008-12-03 AGC Flat Glass Europe SA Fireproof glazing

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
朱洪法主编: "《催化剂手册》", 31 August 2008, 金盾出版社 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

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