CN102797030A - Gypsum whisker preparation method - Google Patents
Gypsum whisker preparation method Download PDFInfo
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- CN102797030A CN102797030A CN2012102685733A CN201210268573A CN102797030A CN 102797030 A CN102797030 A CN 102797030A CN 2012102685733 A CN2012102685733 A CN 2012102685733A CN 201210268573 A CN201210268573 A CN 201210268573A CN 102797030 A CN102797030 A CN 102797030A
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- gypsum
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Abstract
The invention discloses a gypsum whisker preparation method which is implemented concretely through the following steps of: adding a special crystallizing agent into ammonium chloride (or ammonium nitrate) fluid so as to obtain a medium solution; carrying out size mixing on dihydrate gypsum by using the medium solution; carrying out hydrothermal reaction on the obtained product; and carrying out filtering and drying on the obtained product so as to obtain semi-hydrated gypsum whiskers. The method disclosed by the invention can achieve the effects that: the reaction condition is mild, the processing equipment is simple, and the investment is small; the method is large in operation elasticity, and easy to realize industrialized production; and the length-diameter ratio of a whisker is large and can reach 50-200, therefore, the quality of the whisker is high.
Description
Technical field
The invention belongs to Chemicals production, new chemical materials field.The present invention relates to a kind of preparation method of crystal whisker of gypsum; More particularly, be that to add special crystallization in motion agent with ammonium chloride (or an ammonium nitrate) liquid be medium solution, dihydrate gypsum is sized mixing with medium solution; Carry out hydro-thermal reaction then, obtain the semi-hydrated gypsum whisker through filtration, drying again.
Background technology
Crystal whisker of gypsum, another name: gypsum fiber, calcium sulfate crystal whiskers; Length-to-diameter ratio: more than 20.Crystal whisker of gypsum have preferably dispersed and with the compound ability of other materials, strongthener is done by section in multiple inorganic, organic gel gel material; Have performances such as good friction, insulation, heat insulation, fire prevention, non-conductor insulation, can be used as friction materials, heat preserving and insulating material and fire prevention (fire-retardant) material etc.; Have fibrous texture, can be applicable to aspects such as papermaking, coating, rubber, plastics.
The preparation method of crystal whisker of gypsum mainly is a hydrothermal method at present.The technical process of this method is: dihydrate gypsum → grinding → slip → hydro-thermal reaction → filtration → drying → semi-hydrated gypsum whisker → calcination → anhydrite whisker.Wherein, gypsum raw material can be chosen wantonly, but calcium sulphate content is more preferably greater than 95%, and fineness best 80% requires to have basically no detrimental impurity less than 60 orders.The massfraction of slip is controlled at 5%-10% usually, and massfraction is important controlling factor.Hydrothermal temperature is generally 105-150 ℃ of scope or higher; Pressure is 202.65-506.63k Pa, and time 0.5-8h should be incubated for some time under optimal reaction temperature; So that all calcium sulfate all are transformed into whisker, become behind the fibre immediately loose whisker with excessive water sepn.General employing press filtration, temperature must not be lower than 100 ℃ during press filtration, and filter cake is dry immediately, and carries out stabilization treatment while hot, just processes the semi-hydrated gypsum whisker, and its average L/d can reach 60--100.With (400-600 ℃) roasting at high temperature of this semi-hydrated gypsum whisker, the insoluble anhydrite whisker of dead roasting, this product can keep stable for a long time, when having moisture to exist, also is difficult for returning back to hydrated state.This method can be processed crystal whisker of gypsum to some depleted dihydrate gypsums, but hydro-thermal reaction needs comparatively high temps and big pressure.
The calcium sulfate crystal whiskers related patent U.S. Patent No. is following:
It is the CaSO4 whisker and preparation method thereof of raw material with the desulfurated plaster that CN101550602 discloses a kind of.Its technical scheme is: earlier with desulfurated plaster, water and medium crystallization agent thorough mixing, form suspension liquid, wherein: the desulfurated plaster mass concentration is 1～8%, and the medium crystallization agent mass concentration is 5～20%; Be under 120～210r/min condition at normal pressure, 100～128 ℃ and stir speed (S.S.) again, or above-mentioned suspension liquid stirred 1～3 hour that the calcium sulfate crystal whiskers that adds suspension liquid quality 0.5～1% is as crystal seed; Reacted 1～3 hour; Add properties-correcting agent, or above-mentioned suspension liquid was stirred 3～8 hours, directly add properties-correcting agent; The add-on of properties-correcting agent is 0.4～1% of suspension liquid quality, stirs 0.5～1 hour; Through suction filtration, washing and three sections dryings, can obtain three kinds of dissimilar calcium sulfate crystal whiskers then.
CN1598083 the present invention is a kind of Preparation methods of gypsum whiskers method; Whole production is a raw material with plaster stone (CaSO42H2O) and water, through raw material preparation, building-up reactions, dehydrate and an operation such as refining and edulcoration, it is characterized in that the effective content of selected raw material plaster stone reaches more than 95, whiteness is more than 90%; With the mixed plaster stone slip that gets of tap water; After fully emulsified, make it that chemical reaction take place in the adding reactor drum, and then enter into later operation.The calcium sulfate crystal whiskers product performance of utilizing present method to produce are good, with low cost, can widespread uses in every profession and trade, have vast market prospect.
These Preparation methods of gypsum whiskers methods are raw material with natural or by-product terra alba, exist working method control condition harsh and product whiteness is not high, the unequal problem of length-to-diameter ratio, and shortcoming such as production cost height.
Summary of the invention
The object of the present invention is to provide a kind of crystal whisker of gypsum preparation method; It is harsh to change traditional water process for thermosynthesizing control condition; Be difficult to industrialized shortcoming, and the longer crystal whisker of gypsum of production length-to-diameter ratio, to satisfy the demands higher such as papermaking to the crystal whisker of gypsum quality requirements.
Method of the present invention is that to add special crystallization in motion agent with ammonium chloride (or an ammonium nitrate) liquid be medium solution, and dihydrate gypsum is sized mixing with medium solution, carries out hydro-thermal reaction then, again through filter, drying obtains the semi-hydrated gypsum whisker.
The present invention be embodied in following some: (1) is medium with ammonium chloride (or an ammonium nitrate), and ammonium chloride in the circulation fluid (or an ammonium nitrate) concentration reaches 15～35%, makes synthetic dihydrate gypsum slurries more stable.(2) adopt the crystallization in motion agent, the crystallization in motion agent concentration: 1%～5%, promote whisker growth, reach more high length-diameter ratio, and production operation elasticity is increased, be easy to industriallization.(3) the gained calcium sulfate crystal whiskers has high length-diameter ratio and reaches 50-200, and Gao Baiduda 90%, satisfies the demands higher to the crystal whisker of gypsum quality requirements such as papermaking.
The concrete processing condition of crystal whisker preparation method of the present invention:
Ammonium chloride (or an ammonium nitrate) liquid concentration: 15%～35% (massfraction, as follows); 2) crystallization in motion agent concentration: 1%～5%; 3) dihydrate gypsum concentration: 2%～5%; 4) temperature of reaction: 105～130 ℃; 5) time: 0.5～5h.
Characteristics of the present invention: reaction conditions is gentle, and technology is simple; Turndown ratio is big, is prone to suitability for industrialized production; The whisker length-to-diameter ratio is big, and quality is high.
Description of drawings
Accompanying drawing 1 calcium sulfate crystal whiskers design sketch
Embodiment
1, the ammonium chloride solution 100ml of preparation 20% (massfraction); Add the agent of 5g crystallization in motion and process medium solution; Take by weighing the 5g dihydrate gypsum with it wet-milling size mixing, add in the hydrothermal reaction kettle of volume 200ml, put into 120 ℃ of thermostat containers and carry out hydro-thermal reaction 2h; Take out hydrothermal reaction kettle and place pressure release behind the cooling 10min under the room temperature, obtain the semi-hydrated gypsum whisker through filtration, drying again.
2, the ammonium chloride solution 150ml of preparation 20% (massfraction) adds the agent of 7.5g crystallization in motion and processes medium solution, and solution is heated to 90 ℃; Take by weighing 5.55g calcium chloride, 6.60g ammonium sulfate dissolves with medium solution; Liquid calcium chloride and ammonium sulfate liquid short mix in the 200ml beaker are stirred, place the pressure kettle that has boiled, the intensification pressure heat-preserving carries out hydro-thermal reaction 1.5h, and quick pressure releasing obtains the semi-hydrated gypsum whisker through filtration, drying again.
3, the ammonium nitrate solution 150ml of preparation 30% (massfraction) adds the agent of 7.5g crystallization in motion and processes medium solution, and solution is heated to 90 ℃; Take by weighing 8.2g nitrocalcite, 6.6g ammonium sulfate dissolves with medium solution; Nitrocalcite liquid and ammonium sulfate liquid short mix in the 200ml beaker are stirred, place the pressure kettle that has boiled, the intensification pressure heat-preserving carries out hydro-thermal reaction 1.5h, and quick pressure releasing obtains the semi-hydrated gypsum whisker through filtration, drying again.
The invention has the beneficial effects as follows: reaction conditions is gentle, and processing unit is simple, invests little; Turndown ratio is big, is prone to suitability for industrialized production; The whisker length-to-diameter ratio is big, can reach 50-200, and quality is high.
Claims (4)
1. crystal whisker of gypsum preparation method is characterized in that: adding special crystallization in motion agent with ammonium chloride (or an ammonium nitrate) liquid is medium solution, and dihydrate gypsum is sized mixing with medium solution, carries out hydro-thermal reaction then, again through filter, drying obtains the semi-hydrated gypsum whisker.
2. according to right 1 described crystal whisker of gypsum preparation method, it is characterized in that: with ammonium chloride (or an ammonium nitrate) is medium, and ammonium chloride in the circulation fluid (or an ammonium nitrate) concentration reaches 15～35%, makes synthetic dihydrate gypsum slurries more stable.
3. according to right 1 described crystal whisker of gypsum preparation method, it is characterized in that: adopt the crystallization in motion agent, the crystallization in motion agent concentration: 1%～5%, promote whisker growth, reach more high length-diameter ratio, and production operation elasticity is increased, be easy to industriallization.
4. according to right 1 described crystal whisker of gypsum preparation method, it is characterized in that: the gained calcium sulfate crystal whiskers has high length-diameter ratio and reaches 50-200, and Gao Baiduda 90%, satisfies the demands higher to the crystal whisker of gypsum quality requirements such as papermaking.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103757705A (en) * | 2013-12-20 | 2014-04-30 | 淮南市明月环保科技有限责任公司 | Preparation method of anhydrous calcium sulfate whisker |
| CN104030648A (en) * | 2014-06-09 | 2014-09-10 | 孙红芳 | Light fireproof insulation type composite panel |
| CN103757705B (en) * | 2013-12-20 | 2016-11-30 | 淮南市明月环保科技有限责任公司 | A kind of preparation method of anhydrous calcium sulfate whisker |
| CN107059134A (en) * | 2017-03-21 | 2017-08-18 | 东南大学 | A kind of method that crystal whisker of gypsum is prepared under normal pressure |
| CN108265335A (en) * | 2018-01-19 | 2018-07-10 | 北京工业大学 | A kind of semi-hydrated gypsum whisker and preparation method thereof |
| CN109137084A (en) * | 2018-09-10 | 2019-01-04 | 昆明理工大学 | A kind of method of salting out method production Dihydrate gypsum whiskers |
| CN109306261A (en) * | 2017-07-26 | 2019-02-05 | 刘若慧 | A kind of friction material |
| CN115924952A (en) * | 2022-12-14 | 2023-04-07 | 西南科技大学 | Anhydrite powder, gypsum whisker and preparation method thereof |
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| JPS5333319B2 (en) * | 1975-01-31 | 1978-09-13 | ||
| JPS59137317A (en) * | 1983-01-27 | 1984-08-07 | Toyo Soda Mfg Co Ltd | Manufacture of needlelike alpha-hemihydrate gypsum |
| CN101219781A (en) * | 2007-12-07 | 2008-07-16 | 苏兆祥 | Clean production of phosphate and phosphoric acid with low ore grade phosphorus ore hydrochloric acid circulation |
| CN101575106A (en) * | 2008-05-05 | 2009-11-11 | 朱作远 | Coproduction technology of calcium sulphate crystal whiskers and magnesium hydrate crystal whiskers by plaster-ammonium rotation method |
| CN101671848A (en) * | 2009-09-28 | 2010-03-17 | 清华大学 | Preparation method of high length-diameter ratio anhydrous calcium sulfate whisker |
| CN101736403A (en) * | 2009-12-14 | 2010-06-16 | 昆明理工大学 | Method for preparing calcium sulfate crystal whiskers by using impurity-containing gypsum as raw material |
| 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 |
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2012
- 2012-07-25 CN CN2012102685733A patent/CN102797030A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JPS5333319B2 (en) * | 1975-01-31 | 1978-09-13 | ||
| JPS59137317A (en) * | 1983-01-27 | 1984-08-07 | Toyo Soda Mfg Co Ltd | Manufacture of needlelike alpha-hemihydrate gypsum |
| CN101219781A (en) * | 2007-12-07 | 2008-07-16 | 苏兆祥 | Clean production of phosphate and phosphoric acid with low ore grade phosphorus ore hydrochloric acid circulation |
| CN101575106A (en) * | 2008-05-05 | 2009-11-11 | 朱作远 | Coproduction technology of calcium sulphate crystal whiskers and magnesium hydrate crystal whiskers by plaster-ammonium rotation method |
| CN101671848A (en) * | 2009-09-28 | 2010-03-17 | 清华大学 | Preparation method of high length-diameter ratio anhydrous calcium sulfate whisker |
| CN101736403A (en) * | 2009-12-14 | 2010-06-16 | 昆明理工大学 | Method for preparing calcium sulfate crystal whiskers by using impurity-containing gypsum as raw material |
| 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 |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103757705A (en) * | 2013-12-20 | 2014-04-30 | 淮南市明月环保科技有限责任公司 | Preparation method of anhydrous calcium sulfate whisker |
| CN103757705B (en) * | 2013-12-20 | 2016-11-30 | 淮南市明月环保科技有限责任公司 | A kind of preparation method of anhydrous calcium sulfate whisker |
| CN104030648A (en) * | 2014-06-09 | 2014-09-10 | 孙红芳 | Light fireproof insulation type composite panel |
| CN104030648B (en) * | 2014-06-09 | 2016-03-09 | 孙红芳 | A kind of lightweight fireproof insulating type composition board |
| CN107059134A (en) * | 2017-03-21 | 2017-08-18 | 东南大学 | A kind of method that crystal whisker of gypsum is prepared under normal pressure |
| CN109306261A (en) * | 2017-07-26 | 2019-02-05 | 刘若慧 | A kind of friction material |
| CN108265335A (en) * | 2018-01-19 | 2018-07-10 | 北京工业大学 | A kind of semi-hydrated gypsum whisker and preparation method thereof |
| CN109137084A (en) * | 2018-09-10 | 2019-01-04 | 昆明理工大学 | A kind of method of salting out method production Dihydrate gypsum whiskers |
| CN109137084B (en) * | 2018-09-10 | 2021-06-18 | 昆明理工大学 | Method for producing calcium sulfate dihydrate crystal whisker by salting-out method |
| CN115924952A (en) * | 2022-12-14 | 2023-04-07 | 西南科技大学 | Anhydrite powder, gypsum whisker and preparation method thereof |
| CN115924952B (en) * | 2022-12-14 | 2024-05-03 | 西南科技大学 | Anhydrite powder, gypsum whisker and preparation method thereof |
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Application publication date: 20121128 |