CN105332058A - Method for preparing gypsum whiskers for papermaking from phosphogypsum under normal pressure in circulating dissolving method - Google Patents
Method for preparing gypsum whiskers for papermaking from phosphogypsum under normal pressure in circulating dissolving method Download PDFInfo
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- CN105332058A CN105332058A CN201510748188.2A CN201510748188A CN105332058A CN 105332058 A CN105332058 A CN 105332058A CN 201510748188 A CN201510748188 A CN 201510748188A CN 105332058 A CN105332058 A CN 105332058A
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- CN
- China
- Prior art keywords
- phosphogypsum
- normal pressure
- lysate
- gypsum
- whisker
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
- C30B29/62—Whiskers or needles
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/46—Sulfur-, selenium- or tellurium-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/14—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions the crystallising materials being formed by chemical reactions in the solution
Abstract
The invention discloses a method for preparing gypsum whiskers for papermaking from phosphogypsum under normal pressure in a circulating dissolving method. Under normal pressure, SiO2, GaO, FeO and other elements in phosphogypsum are dissolved and separated through circulating dissolving liquid, and high-quality calcium sulphate whiskers are prepared; under the condition that the PH value of the dissolving liquid is set, the dissolving liquid which goes bag is separated at low temperature under normal pressure, a crystallization promoting agent is added, precipitation and crystallization are performed, and high-quality calcium sulphate whiskers capable of partially replacing paper pulp are prepared through modification. The method is low preparation cost, economical and practical, and industrial waste phosphogypsum can be comprehensively utilized. The calcium sulphate whiskers prepared through the method are sufficient in crystallization, moderate in crystal, high in whiteness, resistant to high temperature and fine in product, are optical additives for making paper, rubber, friction plate building materials, wall coating and other products, and have wide application and market prospects.
Description
Technical field
The present invention relates to industrial enterprise's solid waste recycling and Preparation Technique of Powders field, the dissolution method that specifically circulates under a kind of phosphogypsum normal pressure produces the method for gypsum for paper whisker.
Background technology
Phosphogypsum is the waste residue emitted during phosphorous chemical industry enterprise produces, processing mode is always stored up for building a dam, the existing volume of cargo in storage in Yunnan Province just crosses more than hundred million tons, the phosphorous chemical industry enterprise quantity discharged in annual Yunnan Province is more than upper kiloton, and a large amount of stackings causes environment, air, water source, forest, massif etc., many-sided pollution; Just there is the stacking pollution problem because of phosphogypsum in chemical plant, Yunnan, causes plant shutdowns, and related personnel enters the environmental protection event caused a sensation throughout the country of punishment; Take over the land for use, build a dam, transport, manage, the expense of great number makes enterprise can't bear the heavy load, a lot of enterprises long-term loss; A number middle or small phosphorous chemical industry enterprise in Yunnan just has to close down because processed phosphogypsum solution never, many the chemical enterprises in the whole nation are also according to the mineral constituent characteristic of phosphogypsum, research and develop all kinds of building material product, as phosphogypsum making burn-free bricks, phosphogypsum gas concrete product etc., but because of in phosphogypsum about 20% the active processing cost of silicon-dioxide too high, so tret is few in using as building materials, be worth low, be not enough to the practical problems solving enterprise; The cost pain of the superfluous Ye Shi enterprise of chemical enterprise hydrochloric acid, and adopt phosphogypsum hydrochloric acid method to prepare calcium sulfate crystal whiskers there is the low value-added height of production cost, operation strategies extensively waits many advantages, the paper pulp breach nearly 50% that China is annual, need a large amount of import, as crystal whisker of gypsum is applied in papermaking, papermaking enterprise cost will be made to decline to a great extent, fill up the breach of paper pulp deficiency, the fiber be applied in the goods such as rubber, plastics, friction plate adds the volume of cargo in storage substituting and will effectively cut down phosphogypsum, can timber be saved simultaneously, improve environmental quality.
Summary of the invention
The dissolution method that circulates under the object of the present invention is to provide a kind of phosphogypsum normal pressure produces the method for gypsum for paper whisker, adopts phosphogypsum as the raw material preparing calcium sulfate crystal whiskers, has accomplished the regeneration of Industrial Solid Waste resource; The dissolution extraction liquid cost of preparation is low, and production technique is new, and technical process is short, and equipment is simple, and less investment, energy consumption is low, can accomplish in production process without discharging of waste liquid.
For achieving the above object, the invention provides following technical scheme:
The dissolution method that circulates under phosphogypsum normal pressure produces a method for gypsum for paper whisker, comprises following steps:
1) preparation is used for the lysate of dissolved phosphorus gypsum;
2) phosphogypsum is put in proportion in the lysate after heating, stir at ambient pressure and make it dissolve, obtain mixed solution;
3) adding crystallization promoter according to demand makes itself and mixed solution merge;
4) by sedimentation and filtering separation insolubles;
5) cool, crystallization goes out calcium sulfate crystal whiskers;
6) mixed solution after separating calcium sulphate whisker is regulated pH value, again recycle as lysate;
7) isolated calcium sulfate crystal whiskers spray modification solvent, realizes the modification of thing phase, and the retention improving calcium sulfate crystal whiskers makes its suitable papermaking add.
As the further scheme of the present invention: the lysate in described step 1 is made up of the material of following weight part: concentration is hydrochloric acid 30-85 parts, 5-15 parts, the ammonium sulfate of concentration 95%, 2-10 parts, the hydrogen peroxide of concentration 5% of 8%-45%, the concentration of lysate is between 10%-40%, and pH value is between 0.2-6.
As the present invention's further scheme: in described step 1, phosphogypsum is the high silicon of Yunnan part phosphorous chemical industry enterprise discharge, fluorine-containing all kinds of phosphogypsums.
As the present invention's further scheme: the crystallization promoter in described step 3 is magnesium salts solvent.
As the present invention's further scheme: the modification solvent in described step 7 is strong base solution, comprise Ca (OH)
2solution, Na
2sO
4solution and Na
2o solution.
As the present invention's further scheme: the acid being used for regulating ph value of mixture in described step 6 is hydrochloric acid or sulfuric acid, the alkali being used for regulating ph value of mixture is Na
2o or NH
3-H
2o, obtains the lysate that pH value is 0.2-6 after adjustment.
As the present invention's further scheme: in described step 2, the solid-to-liquid ratio of phosphogypsum and lysate is 1:5-1:8, the Heating temperature of lysate is 50-120 DEG C, pulp potential value is between MV150-500, and stirring the miscible reaction times is 3-30min, and the ph value of mixture of miscible rear gained is 2-8.
Compared with prior art, the invention has the beneficial effects as follows: the present invention with Industrial Solid Waste phosphogypsum for raw materials for production, adopt the waste ardealite of phosphorous chemical industry enterprise discharge at ambient pressure with the dissolving liquid dissolves of circulation, the manufacture of turning waste into wealth of the various mineral constituents in separation of phosphogypsum goes out the calcium sulfate crystal whiskers of multi-usage, high-quality; The present invention changes the surface properties of thing phase by the spray attachment of corresponding properties solvent, make its suitable additive as papermaking material, the Calcium Sulfate Whiskers produced, length are all suitable for substituting of papermaking and add, and technical process is short, and facility investment is few; The present invention's controlled Sulphuric acid calcium pyroborate reaches required size, and isolated silicon-dioxide has the activity of more than 60%, can directly use in material of construction, is the economical method of comprehensive utilization phosphogypsum; The calcium sulfate crystal whiskers that the present invention prepares has the performance of resistance to more than 1400 degree high temperature, can as the substitute of fibrous matter needed for other mechanicalss; The calcium sulfate crystal whiskers that the present invention is separated by filtration, crystallisation by cooling, washing are prepared after changing, purity is more than 95%, and whiteness is more than 90%, diameter is 300-600um, and length is 100-5000um, and copy paper experiment turnover rate is less than 15%, high temperature resistant, the advantage that production cost is low; Adopt phosphogypsum as the raw material preparing calcium sulfate crystal whiskers, accomplished the regeneration of Industrial Solid Waste resource, the dissolution extraction liquid cost of preparation is low, and production technique is new, technical process is short, and equipment is simple, less investment, energy consumption is low, can accomplish without discharging of waste liquid in production process, has great promotional value.
Embodiment
Be described in more detail below in conjunction with the technical scheme of embodiment to this patent.
The dissolution method that circulates under phosphogypsum normal pressure produces a method for gypsum for paper whisker, comprises following steps:
1) preparation is used for the lysate of dissolved phosphorus gypsum;
2) phosphogypsum is put in proportion in the lysate after heating, stir at ambient pressure and make it dissolve, obtain mixed solution;
3) adding crystallization promoter according to demand makes itself and mixed solution merge;
4) by sedimentation and filtering separation insolubles;
5) cool, crystallization goes out calcium sulfate crystal whiskers;
6) mixed solution after separating calcium sulphate whisker is regulated pH value, again recycle as lysate;
7) isolated calcium sulfate crystal whiskers spray modification solvent, realizes the modification of thing phase, and the retention improving calcium sulfate crystal whiskers makes its suitable papermaking add.
Lysate in described step 1 is made up of the material of following weight part: concentration is hydrochloric acid 30-85 parts, 5-15 parts, the ammonium sulfate of concentration 95%, 2-10 parts, the hydrogen peroxide of concentration 5% of 8%-45%, the concentration of lysate is between 10%-40%, and pH value is between 0.2-6.
In described step 1, phosphogypsum is the high silicon of Yunnan part phosphorous chemical industry enterprise discharge, fluorine-containing all kinds of phosphogypsums.
Crystallization promoter in described step 3 is magnesium salts solvent.
Modification solvent in described step 7 is strong base solution, comprises Ca(OH)
2solution, Na
2sO
4solution and Na
2o solution.
The acid being used for regulating ph value of mixture in described step 6 is hydrochloric acid or sulfuric acid, and the alkali being used for regulating ph value of mixture is Na
2o or NH
3-H
2o, obtains the lysate that pH value is 0.2-6 after adjustment.
In described step 2, the solid-to-liquid ratio of phosphogypsum and lysate is 1:5-1:8, the Heating temperature of lysate is 50-120 DEG C, pulp potential value is between MV150-500, stirring the miscible reaction times is 3-30min, obtaining ph value of mixture after miscible is 2-8, is separated by filtration, purity more than 95%, whiteness more than 90% are prepared in crystallisation by cooling, washing calcium sulfate crystal whiskers after changing, and Calcium Sulfate Whiskers is 300-600um, length is 100-5000um, and copy paper experiment turnover rate is less than 15%.
Embodiment 1
Take the phosphogypsum that street phosphate fertilizer plant of Jinning County two, 100g Kunming stores up, wherein calcium sulphate content 70%, add in the 500 milliliters of lysates prepared, lysate is containing the hydrochloric acid 150g of 31% concentration, the hydrogen peroxide 10ml of 3% concentration, tap water 340ml, lysate Heating temperature is 60 DEG C, pH value is 0.2, pulp potential is MV150, stirs 10min, add 3g magnesium oxide with the speed of 30 times/min, stir 5min suction filtration again and obtain liquid 380ml, the impurity 30g such as dried white residue, liquid leaves standstill naturally cooling 3h, filters to obtain calcium sulfate crystal whiskers 56g; After testing: sulfate dihydrate calcium contents is greater than 95%, 56g crystal whisker of gypsum through with 100ml content Ca (OH)
2: the solution spraying washing modification of water=1:10, obtained desired product, whiteness is greater than 90%, diameter of whiskers 300-500um, length 2000-5000um.
Embodiment 2
Take the phosphogypsum of 100g Yuxi river and mountain phosphate fertilizer plant, wherein calcium sulphate content 68%, add in the 500ml lysate prepared, lysate is containing the hydrochloric acid 140g of 31% concentration, the hydrogen peroxide 10ml of 3% concentration, ammonium sulfate 20g, tap water 340ml, Heating temperature is 100 DEG C, pH value is 0.25, pulp potential is MV180, 10min is stirred with the speed of 30 times/min, add 3g magnesium sulfate, stir 5min again, suction filtration obtains liquid 360ml, the impurity 30g such as dry rear white residue, liquid is forced to be cooled to 10 DEG C, 30min consuming time, filter to obtain calcium sulfate crystal whiskers 59g, after testing: sulfate dihydrate calcium contents is greater than 95%, 59g crystal whisker of gypsum is through being Na with 100ml content
2o:Na
2sO
4: the mixing solutions spray washing modification of water=1:0.5:10, obtained desired product, whiteness is greater than 90%, diameter of whiskers 200-500um, length 1500-5000um.
Above the better embodiment of this patent is explained in detail, but this patent is not limited to above-mentioned embodiment, in the ken that one skilled in the relevant art possesses, various change can also be made under the prerequisite not departing from this patent aim.
Claims (7)
1. the dissolution method that circulates under phosphogypsum normal pressure produces a method for gypsum for paper whisker, it is characterized in that, comprises following steps:
1) preparation is used for the lysate of dissolved phosphorus gypsum;
2) phosphogypsum is put in proportion in the lysate after heating, stir at ambient pressure and make it dissolve, obtain mixed solution;
3) adding crystallization promoter according to demand makes itself and mixed solution merge;
4) by sedimentation and filtering separation insolubles;
5) cool, crystallization goes out calcium sulfate crystal whiskers;
6) mixed solution after separating calcium sulphate whisker is regulated pH value, again recycle as lysate;
7) isolated calcium sulfate crystal whiskers spray modification solvent, realizes the modification of thing phase, improves the retention of calcium sulfate crystal whiskers.
2. the dissolution method that circulates under phosphogypsum normal pressure according to claim 1 produces the method for gypsum for paper whisker, it is characterized in that, lysate in described step 1 is made up of the material of following weight part: concentration is hydrochloric acid 30-85 parts, 5-15 parts, the ammonium sulfate of concentration 95%, 2-10 parts, the hydrogen peroxide of concentration 5% of 8%-45%, the concentration of lysate is 10%-40%, and pH value is 0.2-6.
3. the dissolution method that circulates under phosphogypsum normal pressure according to claim 1 produces the method for gypsum for paper whisker, it is characterized in that, in described step 1, phosphogypsum is the high silicon of Yunnan part phosphorous chemical industry enterprise discharge, fluorine-containing all kinds of phosphogypsums.
4. the dissolution method that circulates under phosphogypsum normal pressure according to claim 1 produces the method for gypsum for paper whisker, it is characterized in that, in described step 2, the solid-to-liquid ratio of phosphogypsum and lysate is 1:5-1:8, the Heating temperature of lysate is 50-120 DEG C, the miscible reaction times is 3-30min, and miscible rear gained ph value of mixture is 2-8.
5. the dissolution method that circulates under phosphogypsum normal pressure according to claim 1 produces the method for gypsum for paper whisker, and it is characterized in that, the crystallization promoter in described step 3 is magnesium salts solvent.
6. the dissolution method that circulates under phosphogypsum normal pressure according to claim 1 produces the method for gypsum for paper whisker, and it is characterized in that, the modification solvent in described step 7 is strong base solution, comprises Ca (OH)
2solution, Na
2sO
4solution and Na
2o solution.
7. the dissolution method that circulates under phosphogypsum normal pressure according to claim 1 produces the method for gypsum for paper whisker, it is characterized in that, the acid being used for regulating ph value of mixture in described step 6 is hydrochloric acid or sulfuric acid, and the alkali being used for regulating ph value of mixture is Na
2o or NH
3-H
2o, obtains the lysate that pH value is 0.2-6 after adjustment.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510748188.2A CN105332058B (en) | 2015-11-06 | 2015-11-06 | The method that dissolution method produces gypsum for paper whisker is recycled under ardealite normal pressure |
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|---|---|---|---|
| CN201510748188.2A CN105332058B (en) | 2015-11-06 | 2015-11-06 | The method that dissolution method produces gypsum for paper whisker is recycled under ardealite normal pressure |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106758499A (en) * | 2017-03-23 | 2017-05-31 | 长沙理工大学 | A kind of method for improving hot-pressing type bedding paper heat resistance |
| CN107190325A (en) * | 2017-05-09 | 2017-09-22 | 武汉理工大学 | A kind of method that utilization industrial by-product ardealite prepares anhydrous calcium sulfate whisker |
| CN107557870A (en) * | 2017-09-08 | 2018-01-09 | 云南磷化集团有限公司 | A kind of method with preparing calcium sulphate whiskers from ardealite |
| CN111994938A (en) * | 2020-08-31 | 2020-11-27 | 湖北工业大学 | Method for preparing pure calcium sulfate whisker from carbide slag modified phosphogypsum |
| CN115043619A (en) * | 2022-06-21 | 2022-09-13 | 宜都兴发化工有限公司 | Preparation method of self-gelling fiber composite material |
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| CN101311355A (en) * | 2008-04-24 | 2008-11-26 | 云南民族大学 | Process for preparing calcium sulphate whiskers from ardealite |
| CN102383179A (en) * | 2011-10-09 | 2012-03-21 | 昆明理工大学 | Method of comprehensive utilization of industrial waste acid and ardealite |
| CN104562180A (en) * | 2015-01-07 | 2015-04-29 | 西南科技大学 | Method for preparing calcium sulfate whisker from phosphogypsum |
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2015
- 2015-11-06 CN CN201510748188.2A patent/CN105332058B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101311355A (en) * | 2008-04-24 | 2008-11-26 | 云南民族大学 | Process for preparing calcium sulphate whiskers from ardealite |
| CN102383179A (en) * | 2011-10-09 | 2012-03-21 | 昆明理工大学 | Method of comprehensive utilization of industrial waste acid and ardealite |
| CN104562180A (en) * | 2015-01-07 | 2015-04-29 | 西南科技大学 | Method for preparing calcium sulfate whisker from phosphogypsum |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106758499A (en) * | 2017-03-23 | 2017-05-31 | 长沙理工大学 | A kind of method for improving hot-pressing type bedding paper heat resistance |
| CN106758499B (en) * | 2017-03-23 | 2019-01-22 | 长沙理工大学 | A method of improving hot-pressing type bedding paper heat resistance |
| CN107190325A (en) * | 2017-05-09 | 2017-09-22 | 武汉理工大学 | A kind of method that utilization industrial by-product ardealite prepares anhydrous calcium sulfate whisker |
| CN107190325B (en) * | 2017-05-09 | 2019-10-25 | 武汉理工大学 | A method of anhydrous calcium sulfate whisker is prepared using industrial by-product ardealite |
| CN107557870A (en) * | 2017-09-08 | 2018-01-09 | 云南磷化集团有限公司 | A kind of method with preparing calcium sulphate whiskers from ardealite |
| CN111994938A (en) * | 2020-08-31 | 2020-11-27 | 湖北工业大学 | Method for preparing pure calcium sulfate whisker from carbide slag modified phosphogypsum |
| CN111994938B (en) * | 2020-08-31 | 2022-11-18 | 湖北工业大学 | Method for preparing calcium sulfate whisker from calcium carbide slag modified phosphogypsum |
| CN115043619A (en) * | 2022-06-21 | 2022-09-13 | 宜都兴发化工有限公司 | Preparation method of self-gelling fiber composite material |
| CN115043619B (en) * | 2022-06-21 | 2023-09-12 | 宜都兴发化工有限公司 | Preparation method of self-gelling fiber composite material |
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