CN1648291A - Process for preparing whisker calcium sulfate - Google Patents
Process for preparing whisker calcium sulfate Download PDFInfo
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- CN1648291A CN1648291A CN 200410084713 CN200410084713A CN1648291A CN 1648291 A CN1648291 A CN 1648291A CN 200410084713 CN200410084713 CN 200410084713 CN 200410084713 A CN200410084713 A CN 200410084713A CN 1648291 A CN1648291 A CN 1648291A
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- calcium sulfate
- whisker
- whisker calcium
- distilled water
- lime emulsion
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Abstract
The preparation process of whisker calcium sulfate includes calcining limestone, slaking and refining, acid-alkali neutralization, filtering, washing, surface treatment and drying. The reaction temperature is controlled to generate whisker calcium sulfate of different length/diameter ratio, and the present invention has whisker yield up to 100 %, easy processing of the waste water produced and environment friendship.
Description
Technical Field
The invention relates to a preparation method of whisker calcium sulfate, in particular to a semi-hydrated, anhydrous and dead-burned calcium sulfate fibrous monocrystal produced by using refined calcium hydroxide slurry and sulfuric acid as raw materials and adopting a novel process and a novel formula.
Background
Whiskers are fine crystalline fibers that are almost ideal as single crystals that grow in a needle shape. Has the characteristics of large length-diameter ratio, no grain boundary and the like. Because the diameter is small, the highly ordered atomic arrangement structure during crystallization hardly contains the structural defects of gaps, dislocation and the like of the conventional material, so that the mechanical strength and the modulus are close to the theoretical values of the complete crystal material, and the mechanical property far exceeds the mechanical property of the common granular filler which is used in large quantity at present. The whisker has a special shape with a large length-diameter ratio, so that the whisker becomes a novel composite material reinforcing agent with excellent mechanical property.
Calcium sulfate whiskers are generally made of gypsum, and the synthesis process of gypsum is a conversion process from granular gypsum to fibrous anhydrous calcium sulfate, and the chemical process is as follows:
the specific descriptions can be seen in U.S. patents US3961105 and US3822340, canadian patents CA1017132 and CA1127374, and chinese patents CN1337369 and CN 1477242.
The whisker calcium sulfate synthesized by the hydrothermal method has the defects that the conversion rate is difficult to reach 100 percent, and the impurity content is high.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a whisker calcium sulfate product with the whisker yield of 100% and the high length-diameter ratio capable of being accurately controlled.
The invention aims to be realized by the following technical scheme:
the invention relates to the preparation of lime concentrate, which comprises limestone calcining, slaking and refining processes. The invention also relates to an acid-base neutralization reaction, which comprises the steps of filtering, washing, surface treatment and drying to obtain the whisker calcium sulfate product.
The invention is characterized in that acid-base neutralization reaction is utilized to generate whisker calcium sulfate with different length-diameter ratios at different reaction temperatures. The reaction formula is as follows:
(1) formula (II)
(2) Formula (II)
(3) Formula (II)
The preparation method sequentially comprises the following steps:
A、CaCO3putting the mixture into a resistance furnace, and controlling the temperature to be 850-1200 ℃ to obtain white CaO;
B. then putting distilled water and CaO into a reactor together to be sufficiently digested, and removing blocky particles to obtain refined lime emulsion;
C. and heating the obtained refined lime emulsion to 45-135 ℃ in a reactor, injecting equimolar sulfuric acid solution, stirring for 10-90 min to allow the refined lime emulsion to react fully, and separating, washing, performing surface treatment and drying to obtain the required whisker calcium sulfate.
And B, removing blocky particles from the suspension which is completely digested in the step B by a 120-mesh sieve.
The invention obtains the crystalwhisker calcium sulfate product through limestone calcining, slaking and refining processes and an acid-base neutralization reaction, which comprises the processes of filtering, washing, surface treatment and drying. The controllable whisker calcium sulfate with different length-diameter ratios is generated by controlling different reaction temperatures, the yield of the prepared whisker reaches 100 percent, and the wastewater is easy to treat and is beneficial to environmental protection.
Drawings
FIG. 1 is a flow chart of the preparation process of whisker calcium sulfate of the invention;
FIG. 2 is a photomicrograph of whisker calcium sulfate prepared by the process of the invention;
Detailed Description
How this invention can be carried out is further illustrated by the following specific examples:
example 1
Mixing CaCO3Putting 1000g of limestone with the content of more than 98% into a resistance furnace, controlling the temperature at 850-1200 ℃ to obtain white CaO, then putting 3000ml of distilled water and the CaO into an enamel barrel together for full digestion, sieving the digested suspension with a 120-mesh sieve, and removing blocky particles to obtain the refined lime emulsion. Heating the obtained refined lime emulsion to 95 deg.C in a jacketed glass reactor, and injecting equimolar sulfuric acid solutionAnd stirred for 60 minutes to allow the reaction to proceed sufficiently, the reaction solution was separated using a filtration flask, and the obtained sample was observed under a microscope, as shown in FIG. 2.
The industrial product whisker calciumsulfate needs to be modified by different surface treatment agents according to different application objects so as to be better fused with a matrix material.
Example 2
The conditions were the same as in example 1 except that the reaction temperature of the neutralization reaction was 45 ℃.
Example 3
The conditions were the same as in example 1 except that the reaction temperature of the neutralization reaction was 80 ℃.
Example 4
The conditions were the same as in example 1 except that the reaction temperature for the neutralization reaction was 110 ℃.
Example 5
The conditions were the same as in example 1 except that the reaction temperature of the neutralization reaction was 125 ℃.
Example 6
The conditions were the same as in example 1 except that the reaction temperature for the neutralization reaction was 135 ℃.
The whisker calcium sulfate product prepared by the process method has the following properties:
the performance comparison of the whisker calcium sulfate synthesized by the existing hydrothermal method and the whisker calcium sulfate synthesized by the method of the invention is shown in the following table:
| conversion rate% | Content of impurities | Aspect ratio | |
| The existing synthetic method | ＜93 | Is provided with | Is not adjustable |
| The synthesis method of the invention | 100 | Is free of | Is adjustable |
The waste water of the invention is clear liquid, does not contain harmful components, is slightly acidic, is neutralized to be neutral by calcium hydroxide liquid, can be discharged through a three-stage sedimentation tank, is easy to treat and is beneficial to environmental protection.
Claims (2)
1. A preparation method of whisker calcium sulfate sequentially comprises the following steps:
A. mixing CaCO3Putting the mixture into a resistance furnace, controlling the temperature to be 850-1200 ℃ to obtain white BaO, then taking distilled water, putting the distilled water and CaO into a reactor together, fully digesting the distilled water, and removing blocky particles to obtain refined lime emulsion;
C. and heating the obtained refined lime emulsion to 45-135 ℃ in a reactor, injecting equimolar sulfuric acid solution, stirring for 10-90 min to allow the refined lime emulsion to react fully, and separating, washing, performing surface treatment and drying to obtain the required whisker calcium sulfate.
2. The method for preparing whisker calcium sulfate according to claim 1, which is characterized in that: and B, removing blocky particles from the suspension which is completely digested in the step B by a 120-mesh sieve.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100847137A CN1324170C (en) | 2004-11-30 | 2004-11-30 | Process for preparing whisker calcium sulfate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100847137A CN1324170C (en) | 2004-11-30 | 2004-11-30 | Process for preparing whisker calcium sulfate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1648291A true CN1648291A (en) | 2005-08-03 |
| CN1324170C CN1324170C (en) | 2007-07-04 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2004100847137A Expired - Fee Related CN1324170C (en) | 2004-11-30 | 2004-11-30 | Process for preparing whisker calcium sulfate |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100451182C (en) * | 2007-01-23 | 2009-01-14 | 东北大学 | Production of non-metallic material calcium-sulfate whiskers |
| CN100545324C (en) * | 2007-04-16 | 2009-09-30 | 云南常青树化工有限公司 | The preparation method of a kind of calcium sulfate crystal whiskers and phosphoric acid |
| CN101311337B (en) * | 2008-04-25 | 2010-06-16 | 东北大学 | Process for preparing calcium sulphate whiskers by using flue gas desulfurization gypsum |
| CN101550602B (en) * | 2009-05-19 | 2011-10-05 | 武汉科技大学 | CaSO4 crystal whisker with desulfurized gypsum as raw material and preparing method |
| CN102534773A (en) * | 2012-02-02 | 2012-07-04 | 四川万润非金属矿物材料有限公司 | Production method of high-reinforcement modified anhydrous calcium sulfate crystal whiskers |
| CN102618931A (en) * | 2012-04-06 | 2012-08-01 | 江苏省范群干燥设备厂有限公司 | Method for preparing calcium sulfate whiskers |
| CN104499040A (en) * | 2014-12-05 | 2015-04-08 | 上海宝冶钢渣综合开发实业有限公司 | Method for preparing gypsum whisker |
| CN104649310A (en) * | 2013-11-18 | 2015-05-27 | 林琮议 | Manufacturing method of neutral calcium compound and neutral soil |
| CN104692443A (en) * | 2015-03-24 | 2015-06-10 | 枣庄市泰瑞精细化工有限公司 | Manufacturing method using 1,5 naphthalene disulfonic acid reactive mother solution to prepare calcium sulfate |
| CN105112989A (en) * | 2015-10-14 | 2015-12-02 | 科洋环境工程（上海）有限公司 | Preparation method of calcium sulfate whisker |
| CN106241849A (en) * | 2016-06-27 | 2016-12-21 | 枣庄市泰瑞精细化工有限公司 | A kind of method utilizing the waste water producing naphthalenedisulfonic acid to prepare gypsum for cement |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3961105A (en) * | 1972-03-27 | 1976-06-01 | Certain-Teed Products Corporation | Method for the manufacture of coated calcium sulfate whisker fibers |
| 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
- 2004-11-30 CN CNB2004100847137A patent/CN1324170C/en not_active Expired - Fee Related
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100451182C (en) * | 2007-01-23 | 2009-01-14 | 东北大学 | Production of non-metallic material calcium-sulfate whiskers |
| CN100545324C (en) * | 2007-04-16 | 2009-09-30 | 云南常青树化工有限公司 | The preparation method of a kind of calcium sulfate crystal whiskers and phosphoric acid |
| CN101311337B (en) * | 2008-04-25 | 2010-06-16 | 东北大学 | Process for preparing calcium sulphate whiskers by using flue gas desulfurization gypsum |
| CN101550602B (en) * | 2009-05-19 | 2011-10-05 | 武汉科技大学 | CaSO4 crystal whisker with desulfurized gypsum as raw material and preparing method |
| CN102534773A (en) * | 2012-02-02 | 2012-07-04 | 四川万润非金属矿物材料有限公司 | Production method of high-reinforcement modified anhydrous calcium sulfate crystal whiskers |
| CN102534773B (en) * | 2012-02-02 | 2015-04-08 | 四川万润非金属矿物材料有限公司 | Production method of high-reinforcement modified anhydrous calcium sulfate crystal whiskers |
| CN102618931B (en) * | 2012-04-06 | 2015-04-22 | 江苏省范群干燥设备厂有限公司 | Method for preparing calcium sulfate whiskers |
| CN102618931A (en) * | 2012-04-06 | 2012-08-01 | 江苏省范群干燥设备厂有限公司 | Method for preparing calcium sulfate whiskers |
| CN104649310A (en) * | 2013-11-18 | 2015-05-27 | 林琮议 | Manufacturing method of neutral calcium compound and neutral soil |
| CN104499040A (en) * | 2014-12-05 | 2015-04-08 | 上海宝冶钢渣综合开发实业有限公司 | Method for preparing gypsum whisker |
| CN104499040B (en) * | 2014-12-05 | 2017-06-30 | 上海宝冶钢渣综合开发实业有限公司 | A kind of method for preparing crystal whisker of gypsum |
| CN104692443A (en) * | 2015-03-24 | 2015-06-10 | 枣庄市泰瑞精细化工有限公司 | Manufacturing method using 1,5 naphthalene disulfonic acid reactive mother solution to prepare calcium sulfate |
| CN105112989A (en) * | 2015-10-14 | 2015-12-02 | 科洋环境工程（上海）有限公司 | Preparation method of calcium sulfate whisker |
| CN105112989B (en) * | 2015-10-14 | 2017-09-12 | 科洋环境工程（上海）有限公司 | A kind of preparation method of calcium sulfate crystal whiskers |
| CN106241849A (en) * | 2016-06-27 | 2016-12-21 | 枣庄市泰瑞精细化工有限公司 | A kind of method utilizing the waste water producing naphthalenedisulfonic acid to prepare gypsum for cement |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1324170C (en) | 2007-07-04 |
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Granted publication date: 20070704 Termination date: 20091230 |