CN1699638A - Process for preparing calcium sulfate crystal whisker material - Google Patents
Process for preparing calcium sulfate crystal whisker material Download PDFInfo
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- CN1699638A CN1699638A CN 200410026160 CN200410026160A CN1699638A CN 1699638 A CN1699638 A CN 1699638A CN 200410026160 CN200410026160 CN 200410026160 CN 200410026160 A CN200410026160 A CN 200410026160A CN 1699638 A CN1699638 A CN 1699638A
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- whisker
- gypsum
- calcium sulfate
- sulfate crystal
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Abstract
The present invention relates to a preparation process of calcium sulfate crystal whisker. Gypsum is used as raw material and water as medium. After three processes of mixing, synthesis and drying, the product is obtained. The control of the process is easy, operation simple, production period short, production cost low, production purity high, quality stable and yield high. It can be widely used in the industries of plastics, rubber, adhesives, wearing material, coating, thermo-insulation material, environment engineering and light architecture material, etc.
Description
Technical field
The present invention relates to a kind of preparation technology of calcium sulfate crystal whiskers material.
Background technology
Whisker is that a kind of diameter of generating with the monocrystalline form under the manual control condition has only several microns, length that tens microns filamentary material is arranged, it has characteristics such as length-to-diameter ratio is big, no grain boundary, just because of this intrinsic integrity of whisker, its intensity is not limited by the strictness of surface integrity, is endowed with polycrystalline fibre, glass fibre and compares very tough and tensile character.The kind of crystal whisker materials is a lot of at present, and calcium sulfate crystal whiskers is exactly one of them.As a kind of novel crystal whisker materials, calcium sulfate crystal whiskers has intensity height, high temperature resistant, resist chemical, good toughness, easily carries out advantages such as the avidity of polymkeric substance such as surface treatment and rubber, plastics is strong, can be widely used in industries such as plastics, rubber, caking agent, friction materials, coating, paint, lagging material, environmental engineering and light building material, and its price is very cheap, has wide application and market outlook.
Summary of the invention
The purpose of this invention is to provide a kind of Preparation methods of gypsum whiskers technology.
Purpose of the present invention can realize by following measure:
A kind of Preparation methods of gypsum whiskers technology may further comprise the steps: 1. gypsum and water are mixed according to a certain percentage, make slip; 2. above-mentioned slip is placed autoclave, the temperature and pressure and the reaction times of control reactor; 3. after question response was finished, drying under reduced pressure promptly got calcium sulfate crystal whiskers.
1. middle gypsum of described step and water are with 1: 1-1: 10 mixed.
Described step temperature of reaction 2. is 70-250 ℃.
Described step reaction pressure 2. is 1.0-0.5MPa.
The described step reaction times 2. is 1-10 hour.
Described step 3. drying pressure is the 0.1-1.5 normal atmosphere; Be 1-5 hour time of drying.
The present invention has the following advantages:
1, the present invention is a raw material with the gypsum, is medium with water, makes granular plaster stone transform into the anhydrous calciumsulphate crystal that fiber presses, and its cost is low, technology simple and purity height, the yield of product are big.
2, technology of the present invention is easy to control, easy and simple to handle, preparation cycle weak point, is easy to accomplish scale production.
3, the present invention is moderate to the performance requriements of equipment, constant product quality.
Embodiment
With plaster stone and water in 1: 1-1: 10 ratio thorough mixing is made slip; Again above-mentioned slip is placed autoclave, the temperature of control reactor: 70-250 ℃, reaction pressure: 0.1-1.0MPa and reaction times: 0.5-10 hour, after question response was finished, the pressure that reduces reactor promptly got calcium sulfate crystal whiskers to dry 1-5 hour of 0.1-1.5 normal atmosphere.Crystal whisker products is accredited as pure phase through X-ray diffraction, and the content of calcium sulfate is 98.5% in the product, and the whisker mean diameter is 0.1-1.0um, and mean length is 10-110um, and yield is 98.0%.
Further specify reaction conditions to the generation of calcium sulfate crystal whiskers and the influence of whisker quality below in conjunction with experimental data.
1, the proportioning ratio of gypsum and water is to the generation of calcium sulfate crystal whiskers and the influence of whisker quality: with CaSO
42H
2O, H
2O is a raw material, processing step operation by above-mentioned embodiment, control reaction temperature: 100 ℃, reaction pressure 1.0MPa: reaction times: 1 hour, change the proportioning raw materials ratio simultaneously, observe of the influence (experimental result see Table 1) of different proportioning raw materials to the whisker generating state:
Table 1 (the proportioning raw materials ratio is to the influence of the calcium sulfate crystal whiskers of generation):
| Sequence number | Raw material | The proportioning raw materials ratio | Whisker becomes situation |
| ????1 | ????CaSO 4·2H 2O∶H 2O | ????1∶1 | There is a small amount of whisker to generate |
| ????2 | ????CaSO 4·2H 2O∶H 2O | ????1∶2.5 | There is the whisker of half to generate approximately |
| ????3 | ????CaSO 4·2H 2O∶H 2O | ????1∶3 | There is the whisker of half to generate approximately |
| ????4 | ????CaSO 4·2H 2O∶H 2O | ????1∶4 | There is the whisker of half to generate approximately |
| ????5 | ????CaSO 4·2H 2O∶H 2O | ????1∶5 | Whisker generates fully |
| ????6 | ????CaSO 4·2H 2O∶H 2O | ????1∶10 | Whisker generates fully |
| ????7 | ????CaSO 4·2H 2O∶H 2O | ????1∶20 | Whisker generates fully |
As can be seen from Table 1, in the proportioning raw materials of gypsum and water, the ratio of water is high more, and the generating state of calcium sulfate crystal whiskers is good more, but the ratio of water is too high, then can cause the waste of water resources, so the proportioning ratio of raw material gypsum and water generally is controlled at 1: 1-1: 10 are advisable.
2, reaction pressure is to the generation of calcium sulfate crystal whiskers and the influence of whisker quality: with CaSO
42H
2O and H
2O was with 1: 5 ratio proportioning, processing step operation by above-mentioned embodiment, control reaction temperature: 100 ℃, reaction times: 2 hours, change reaction pressure simultaneously, observe of the influence (experimental result see Table 2) of different reaction pressures to the whisker generating state:
As can be seen from Table 2, have only when reaction pressure reaches certain degree, just have calcium sulfate crystal whiskers to generate, and reaction pressure is big more, the generating state of calcium sulfate crystal whiskers is good more, and the quality of crystal whisker products is high more.But reaction pressure is excessive, increases the burden of equipment, so reaction pressure should be controlled at 0.1-0.5MPa.
Table 2
| Sequence number | Reaction pressure (KPa) | The whisker shape |
| ????1 | ????144 | There is not whisker to generate |
| ????2 | ????220 | There is not whisker to generate |
| ????3 | ????240 | There is not whisker to generate |
| ????4 | ????260 | There is the good whisker of shape to generate |
| ????5 | ????280 | There is the good whisker of shape to generate |
| ????6 | ????324 | There is the good whisker of shape to generate |
| ????7 | ????344 | There is the good whisker of shape to generate |
| ????8 | ????384 | There is the good whisker of shape to generate |
| ????9 | ????404 | There is the good whisker of shape to generate |
| ????10 | ????424 | There is the good whisker of shape to generate |
| ????11 | ????484 | There is the good whisker of shape to generate |
3, the reaction times is to the generation of calcium sulfate crystal whiskers and the influence of whisker quality: with CaSO
42H
2O and H
2O was with 1: 5 ratio proportioning, processing step operation by above-mentioned embodiment, control reaction temperature: 100 ℃, reaction pressure: 0.5Mpa, change the reaction times simultaneously, observe of the influence (experimental result see Table 3) of different reaction times to the whisker generating state:
Table 3
| Sequence number | Reaction times (hour) | The whisker shape |
| ????1 | ????10 | There is the good whisker of shape to generate |
| ????2 | ????7 | There is the good whisker of shape to generate |
| ????3 | ????6 | There is the good whisker of shape to generate |
| ????4 | ????5 | There is the good whisker of shape to generate |
| ????5 | ????4 | There is the good whisker of shape to generate |
| ????6 | ????3 | There is the good whisker of shape to generate |
| ????7 | ????2 | There is the good whisker of shape to generate |
| ????8 | ????1 | There is the good whisker of shape to generate |
| ????9 | ????0.75 | There is whisker to generate |
| ????10 | ????0.5 | There is not whisker to generate |
From the experiment of table 3 as can be seen, reaction response deficiency of time 1 hour, reaction is not exclusively, almost do not have calcium sulfate crystal whiskers to generate,, react more complete along with the continuous prolongation in reaction times, shape, the quality of the calcium sulfate crystal whiskers that generates are good more, so general selection of reaction times was advisable in 1-10 hour.
4, temperature of reaction is to the generation of calcium sulfate crystal whiskers and the influence of whisker quality: in general, the temperature of reaction solution is high more, and speed of response is fast more, and sulfating reaction is complete more, and the quality of product is good more.So the temperature of reaction solution generally is controlled at 70-250 ℃ and is advisable.
Claims (6)
1, a kind of Preparation methods of gypsum whiskers technology may further comprise the steps: 1. gypsum and water are mixed according to a certain percentage, make slip; 2. above-mentioned slip is placed autoclave, the temperature and pressure and the reaction times of control reactor; 3. after question response was finished, drying under reduced pressure promptly got calcium sulfate crystal whiskers.
2, Preparation methods of gypsum whiskers technology as claimed in claim 1 is characterized in that: 1. middle gypsum of described step and water are with 1: 1-1: 10 mixed.
3, Preparation methods of gypsum whiskers technology as claimed in claim 1 or 2 is characterized in that: described step temperature of reaction 2. is 70-250 ℃.
4, Preparation methods of gypsum whiskers technology as claimed in claim 1 or 2 is characterized in that: described step reaction pressure 2. is 1.0-0.5MPa.
5, Preparation methods of gypsum whiskers technology as claimed in claim 1 or 2 is characterized in that: the described step reaction times 2. is 1-10 hour.
6, Preparation methods of gypsum whiskers technology as claimed in claim 1 or 2 is characterized in that: described step 3. drying pressure is the 0.1-1.5 normal atmosphere; Be 1-5 hour time of drying.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200410026160XA CN1317430C (en) | 2004-05-18 | 2004-05-18 | Process for preparing calcium sulfate crystal whisker material |
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|---|---|---|---|
| CNB200410026160XA CN1317430C (en) | 2004-05-18 | 2004-05-18 | Process for preparing calcium sulfate crystal whisker material |
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| CN1317430C CN1317430C (en) | 2007-05-23 |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101311337B (en) * | 2008-04-25 | 2010-06-16 | 东北大学 | Process for preparing calcium sulphate whiskers by using flue gas desulfurization gypsum |
| CN101319382B (en) * | 2008-06-25 | 2011-04-27 | 国家海洋局天津海水淡化与综合利用研究所 | Calcium sulphate crystal whisker preparation method with sea water bittern as raw material |
| CN102115142A (en) * | 2010-12-31 | 2011-07-06 | 张胜勇 | Method for producing industrial calcium sulfate by producing ardealite |
| CN102212884A (en) * | 2011-05-04 | 2011-10-12 | 上海大学 | Method for preparing calcium sulfate crystal whisker from many kinds of industrial waste residue gypsum serving as raw materials |
| CN102286783A (en) * | 2011-09-30 | 2011-12-21 | 瓮福（集团）有限责任公司 | New method for preparing calcium sulfate whiskers |
| WO2012034404A1 (en) * | 2010-09-15 | 2012-03-22 | 北新集团建材股份有限公司 | Gypsum whisker, enhanced mineral wool sound-absorbing plate containing the same and preparation method thereof |
| CN101311355B (en) * | 2008-04-24 | 2012-05-02 | 云南民族大学 | Process for preparing calcium sulphate whiskers from ardealite |
| CN102776569A (en) * | 2012-07-09 | 2012-11-14 | 泰山医学院 | Method for preparing calcium sulfate crystal whiskers by using natural gypsum |
| CN104313726A (en) * | 2014-10-10 | 2015-01-28 | 孙红芳 | Preparation method for gypsum fibers |
| CN104328480A (en) * | 2013-09-11 | 2015-02-04 | 江西峰竺新材料科技有限公司 | Preparation method of calcium sulfate whisker |
| CN106319631A (en) * | 2016-08-30 | 2017-01-11 | 湖北永绍科技股份有限公司 | Comprehensive treating and utilizing method of sulfuric acid waste liquor and hydrochloric acid waste liquor |
| CN106350870A (en) * | 2016-08-30 | 2017-01-25 | 湖北永绍科技股份有限公司 | Disposal and utilization method for sulfuric acid waste liquid |
| CN110079865A (en) * | 2019-06-14 | 2019-08-02 | 湘潭大学 | A kind of process of extracting sulfuric acid calcium pyroborate |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1337369A (en) * | 2000-08-03 | 2002-02-27 | 韩晨光 | Gypsum fiber producing process |
| CN1261624C (en) * | 2003-07-08 | 2006-06-28 | 宁夏建筑材料研究院 | Gypsum whisker, its preparation method and application |
-
2004
- 2004-05-18 CN CNB200410026160XA patent/CN1317430C/en not_active Expired - Fee Related
Cited By (20)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101311355B (en) * | 2008-04-24 | 2012-05-02 | 云南民族大学 | Process for preparing calcium sulphate whiskers from ardealite |
| CN101311337B (en) * | 2008-04-25 | 2010-06-16 | 东北大学 | Process for preparing calcium sulphate whiskers by using flue gas desulfurization gypsum |
| CN101319382B (en) * | 2008-06-25 | 2011-04-27 | 国家海洋局天津海水淡化与综合利用研究所 | Calcium sulphate crystal whisker preparation method with sea water bittern as raw material |
| CN102400498B (en) * | 2010-09-15 | 2014-04-09 | 北新集团建材股份有限公司 | Enhanced mineral cotton acoustic board and preparation method thereof |
| WO2012034404A1 (en) * | 2010-09-15 | 2012-03-22 | 北新集团建材股份有限公司 | Gypsum whisker, enhanced mineral wool sound-absorbing plate containing the same and preparation method thereof |
| CN102400498A (en) * | 2010-09-15 | 2012-04-04 | 北新集团建材股份有限公司 | Novel enhanced mineral cotton acoustic board and preparation method thereof |
| CN102115142A (en) * | 2010-12-31 | 2011-07-06 | 张胜勇 | Method for producing industrial calcium sulfate by producing ardealite |
| CN102212884A (en) * | 2011-05-04 | 2011-10-12 | 上海大学 | Method for preparing calcium sulfate crystal whisker from many kinds of industrial waste residue gypsum serving as raw materials |
| CN102286783A (en) * | 2011-09-30 | 2011-12-21 | 瓮福（集团）有限责任公司 | New method for preparing calcium sulfate whiskers |
| CN102286783B (en) * | 2011-09-30 | 2013-05-22 | 瓮福（集团）有限责任公司 | New method for preparing calcium sulfate whiskers |
| CN102776569A (en) * | 2012-07-09 | 2012-11-14 | 泰山医学院 | Method for preparing calcium sulfate crystal whiskers by using natural gypsum |
| CN104328480A (en) * | 2013-09-11 | 2015-02-04 | 江西峰竺新材料科技有限公司 | Preparation method of calcium sulfate whisker |
| CN104328480B (en) * | 2013-09-11 | 2015-08-05 | 江西峰竺新材料科技有限公司 | A kind of calcium sulphate crystal whisker preparation method |
| CN104313726A (en) * | 2014-10-10 | 2015-01-28 | 孙红芳 | Preparation method for gypsum fibers |
| CN106319631A (en) * | 2016-08-30 | 2017-01-11 | 湖北永绍科技股份有限公司 | Comprehensive treating and utilizing method of sulfuric acid waste liquor and hydrochloric acid waste liquor |
| CN106350870A (en) * | 2016-08-30 | 2017-01-25 | 湖北永绍科技股份有限公司 | Disposal and utilization method for sulfuric acid waste liquid |
| CN106319631B (en) * | 2016-08-30 | 2019-02-22 | 湖北永绍科技股份有限公司 | The joint disposal of a kind of sulfuric acid waste and hydrochloride waste utilizes method |
| CN106350870B (en) * | 2016-08-30 | 2019-02-22 | 湖北永绍科技股份有限公司 | A kind for the treatment of and use method of sulfuric acid waste |
| CN110079865A (en) * | 2019-06-14 | 2019-08-02 | 湘潭大学 | A kind of process of extracting sulfuric acid calcium pyroborate |
| CN110079865B (en) * | 2019-06-14 | 2021-03-12 | 湘潭大学 | Process for preparing calcium sulfate crystal whisker |
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| Publication number | Publication date |
|---|---|
| CN1317430C (en) | 2007-05-23 |
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