CN104499040B - A kind of method for preparing crystal whisker of gypsum - Google Patents
A kind of method for preparing crystal whisker of gypsum Download PDFInfo
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- CN104499040B CN104499040B CN201410737390.0A CN201410737390A CN104499040B CN 104499040 B CN104499040 B CN 104499040B CN 201410737390 A CN201410737390 A CN 201410737390A CN 104499040 B CN104499040 B CN 104499040B
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- gypsum
- whisker
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- limestone powder
- sulfuric acid
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- 239000010440 gypsum Substances 0.000 title claims abstract description 45
- 229910052602 gypsum Inorganic materials 0.000 title claims abstract description 45
- 239000013078 crystal Substances 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 25
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 claims abstract description 80
- 235000019738 Limestone Nutrition 0.000 claims abstract description 48
- 239000006028 limestone Substances 0.000 claims abstract description 48
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 35
- 235000011132 calcium sulphate Nutrition 0.000 claims abstract description 32
- 239000000843 powder Substances 0.000 claims abstract description 22
- 239000010802 sludge Substances 0.000 claims abstract description 20
- 238000001914 filtration Methods 0.000 claims abstract description 18
- 238000001035 drying Methods 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000001175 calcium sulphate Substances 0.000 claims abstract description 12
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims abstract description 11
- 229960001763 zinc sulfate Drugs 0.000 claims abstract description 11
- 229910000368 zinc sulfate Inorganic materials 0.000 claims abstract description 11
- 239000003054 catalyst Substances 0.000 claims abstract description 8
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 7
- 239000012467 final product Substances 0.000 claims abstract description 3
- 239000002245 particle Substances 0.000 claims description 7
- 230000008569 process Effects 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims 1
- 239000011701 zinc Substances 0.000 claims 1
- 229910052725 zinc Inorganic materials 0.000 claims 1
- 239000002699 waste material Substances 0.000 abstract description 10
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 238000011161 development Methods 0.000 abstract description 5
- 229910000831 Steel Inorganic materials 0.000 abstract description 3
- 239000010959 steel Substances 0.000 abstract description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical group [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 18
- 229940095672 calcium sulfate Drugs 0.000 description 16
- 239000000463 material Substances 0.000 description 10
- 229910000019 calcium carbonate Inorganic materials 0.000 description 9
- 239000000706 filtrate Substances 0.000 description 5
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 4
- 239000002893 slag Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 238000002425 crystallisation Methods 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000003082 abrasive agent Substances 0.000 description 2
- 229940095564 anhydrous calcium sulfate Drugs 0.000 description 2
- 239000004566 building material Substances 0.000 description 2
- 239000000292 calcium oxide Substances 0.000 description 2
- 235000012255 calcium oxide Nutrition 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 150000004683 dihydrates Chemical class 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 229910010272 inorganic material Inorganic materials 0.000 description 2
- 239000011147 inorganic material Substances 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000010408 sweeping Methods 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 239000002216 antistatic agent Substances 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- ZOMBKNNSYQHRCA-UHFFFAOYSA-J calcium sulfate hemihydrate Chemical compound O.[Ca+2].[Ca+2].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O ZOMBKNNSYQHRCA-UHFFFAOYSA-J 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000013016 damping Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000002389 environmental scanning electron microscopy Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 229940057306 hemihydrate calcium sulfate Drugs 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000003658 microfiber Substances 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000008707 rearrangement Effects 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000009628 steelmaking Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000003053 toxin Substances 0.000 description 1
- 231100000765 toxin Toxicity 0.000 description 1
Abstract
The present invention provides a kind of method for preparing crystal whisker of gypsum, comprises the following steps：1）By the drying of lime stone sludge, limestone powder is obtained；2）Addition dilute sulfuric acid reaction in a certain amount of limestone powder is taken, calcium sulfate is generated；3）By step 2）After the calcium sulfate filtering of middle acquisition, add water and be made into calcium sulphate soln and control its concentration, add zinc sulfate as catalyst, after carrying out hydro-thermal reaction, filtering obtains final product semi-hydrated gypsum whisker；4）After semi-hydrated gypsum whisker is dried, anhydrous gypsum whisker is obtained.A kind of method for preparing crystal whisker of gypsum of the invention, using the lime stone sludge and sulfuric acid waste " turning waste into wealth " that are considered as waste residue that are produced in steel industry, prepares the anhydrous gypsum whisker with excellent properties.The method not only reduces the production cost of crystal whisker of gypsum, and protects environment, and preferably influence is produced with the harmonious development of environment to society.
Description
Technical field
The invention belongs to technical field of inorganic material, and in particular to a kind of method for preparing crystal whisker of gypsum.
Background technology
Whisker atomic structural arrangement high-sequential in crystallization, lacks so that not accommodating and can slacken the larger of crystal
Fall into, such as granular boundary, cavity, dislocation and structure are imperfect, near-complete crystal, cause the intensity of whisker close to material atom
Between valence link theoretical strength, considerably beyond other reinforcing materials for largely using at present.
Crystal whisker of gypsum (i.e. calcium sulfate crystal whiskers Calcium Sulfate Whisker, also known as calcium sulphate micro-fibre, international business
The name of an article is referred to as ONODA-GPF) it is a kind of new inorganic material with very high combination property.Calcium sulfate crystal whiskers be divided into it is anhydrous,
Ban Shui, wherein three kinds of two water, anhydrous calcium sulfate whisker intensity highest.Dihydrate gypsum whiskers when being used more than 110 DEG C from not
To the humidification of whisker, prospects for commercial application is small；Anhydrous and hemihydrate calcium sulfate crystal whisker then has intensity higher and uses valency
Value.
Crystal whisker of gypsum as fibrous monocrystal, with perfect structure, complete profile, specific cross section, stabilization
Size, be a kind of nonmetallic materials for having many properties, generally between 30-100, average length is draw ratio
30-400 μm, average diameter is 1-10 μm.Compared with other chopped fibers, with high temperature resistant, resist chemical, good toughness, intensity
It is high, be easily surface-treated and the affinity of the polymer such as rubber plastic is strong, low toxin, and price is in whisker
In it is relatively low, with the unrivaled ratio of performance to price of other whiskers.The range of application of crystal whisker of gypsum widely, is used primarily in and makes
It is paper industry, composite enhancing, abrasives, Environmental Engineering Material, light building material, heat-barrier material, coating, paint, antistatic
The aspects such as the manufacture of material.At present, the method for preparing crystal whisker of gypsum is more, and various methods have their own characteristics each, but all presence is produced into
This height, product contains the problems such as crystallization water, draw ratio are uneven, and production method control condition is harsh.
Lime stone sludge is produced limestone crushing dedusting damping mud during quick lime is manufactured, and Baosteel is in converter
In steelmaking process, generally require to add a certain amount of quick lime for slag making to adjust slag basicity.Therefore, Baosteel is annual
About 200,000 tons of the lime stone sludge of generation.These lime stone sludge are long-term to pile up, it is also very desirable to which that finding one kind has as discarded object
Effect treatment approach.
The content of the invention
The shortcoming of prior art in view of the above, it is an object of the invention to provide a kind of side for preparing crystal whisker of gypsum
Method, for solving the problems, such as to lack the method for preparing crystal whisker of gypsum using lime stone sludge in the prior art.
In order to achieve the above objects and other related objects, a kind of method for preparing crystal whisker of gypsum of present invention offer, including with
Lower step：
1) lime stone sludge is dried, obtains limestone powder；
Preferably, the main component in the lime stone sludge is calcium carbonate (CaCO3).Carbonic acid in the lime stone sludge
Content >=the 90wt% of calcium.
Preferably, the drying temperature is 450-650 DEG C.Further, the drying temperature is 500 DEG C.
Preferably, the drying time is 2-4 hours.
Preferably, the particle diameter of the limestone powder is 1-10 μm.
2) addition dilute sulfuric acid reaction in a certain amount of limestone powder is taken, calcium sulfate is generated；
Preferably, the dilute sulfuric acid is the sulfuric acid waste of generation in industrial production.
Preferably, the dilute sulfuric acid is aqueous sulfuric acid.Further, the concentration of the dilute sulfuric acid is 5-15wt%.
Preferably, the reaction time is 4 ± 1 hours.Further, the reaction time is 4 hours.
Preferably, in the addition of the dilute sulfuric acid and limestone powder the material of calcium carbonate amount equivalent or excess.From
And calcium carbonate is fully reacted.
3) by step 2) in obtain calcium sulfate filtering after, add water and be made into calcium sulphate soln and control its concentration, add
Used as catalyst, after carrying out hydro-thermal reaction, filtering obtains final product semi-hydrated gypsum whisker to zinc sulfate；
Preferably, the calcium sulphate soln is the calcium sulfate aqueous solution.
Preferably, the concentration of the calcium sulphate soln is controlled to 10-30wt%.
Preferably, the zinc sulfate and the weight ratio of the addition of limestone powder are 1:15-25.
Further, the zinc sulfate and the weight ratio of the addition of limestone powder are 1:20.
Preferably, the condition of the hydro-thermal reaction is：Reaction vessel：Autoclave；Reaction temperature：120±5℃；During reaction
Between：1 ± 0.5 hour.
Further, the condition of the hydro-thermal reaction is：Reaction vessel：Autoclave；Reaction temperature：120℃；During reaction
Between：1 hour.
The principle of the hydro-thermal reaction is：Granular dihydrate gypsum produces structural rearrangement under high temperature hydrothermal condition, brilliant
Body carries out one-dimensional growth, is changed into fibrous semi-hydrated gypsum whisker.
Preferably, the filtering uses strainer filtering.The filter screen is conventional use of 300 mesh nylon leaching net.
4) after semi-hydrated gypsum whisker is dried, anhydrous gypsum whisker is obtained.
Preferably, the condition of the dried process is：Treatment vessel：Drying oven；Treatment temperature：220±10℃；During treatment
Between：1 ± 0.5 hour.
Further, the condition of the dried process is：Treatment vessel：Drying oven；Treatment temperature：220℃；During treatment
Between：1 hour.
Present invention also offers a kind of lime stone sludge according to preparing the method for crystal whisker of gypsum in crystal whisker of gypsum is prepared
Using.
As described above, a kind of method for preparing crystal whisker of gypsum of the invention, goes out from the angle of refuse reclamation, environmental protection
Hair, by using in steel industry produce the lime stone sludge and sulfuric acid waste " turning waste into wealth " that are considered as waste residue, using water
It is high that hot method is translated into quality (whisker length be 100-180 μm, draw ratio 60-100) high, economic value added, range of application
Wide anhydrous gypsum whisker.The anhydrous gypsum whisker stable chemical nature prepared in the present invention, can be widely applied to papermaking
Industry, composite enhancing, abrasives, Environmental Engineering Material, light building material, heat-barrier material, coating, paint, antistatic material
The aspects such as the manufacture of material.A kind of method for preparing crystal whisker of gypsum of the invention, by setting preferred condition so as to overcome preparation
Draw ratio inequality, the problems such as containing the crystallization water that crystal whisker of gypsum is present.A kind of method for preparing crystal whisker of gypsum in the present invention, belongs to
Typical green chemistry process, complies fully with the requirement of the strategy of sustainable development, not only reduces the production cost of crystal whisker of gypsum,
And protect environment, be applied to that socio-economic development will be played certain impetus in actual production, to society with
The harmonious development of environment produces preferably influence.
Brief description of the drawings
Fig. 1 is shown as a kind of process flow diagram of method for preparing crystal whisker of gypsum of the invention
Fig. 2 is shown as the scanning electron microscope sem shape appearance figure of crystal whisker of gypsum in the present invention
Specific embodiment
The present invention is expanded on further with reference to specific embodiment, it should be appreciated that these embodiments are merely to illustrate the present invention
Rather than limit the scope of the invention.
Embodiments of the present invention are illustrated below by way of specific instantiation, those skilled in the art can be by this specification
Disclosed content understands other advantages of the invention and effect easily.The present invention can also be by specific realities different in addition
The mode of applying is embodied or practiced, the various details in this specification can also based on different viewpoints with application, without departing from
Various modifications or alterations are carried out under spirit of the invention.
Raw material and equipment that following examples are used：
1st, raw material
Lime stone sludge, sulfuric acid waste, purchased from upper Hypon smelting slag comprehensive exploitation Industrial Co., Ltd.；Water is running water；
Zinc sulfate, purity 97%, purchased from Wujiang Nan Lin Fine Chemical Co., Ltd.
2nd, equipment
GCF-1L type autoclaves, purchased from Dalian automatic control equipment factory；SX2-4-10 type drying ovens, purchased from Maanshan City's electric furnace
Factory.
Embodiment 1
As shown in figure 1, after lime stone sludge is dried 3 hours at 500 DEG C, obtaining the agstone that particle diameter is for 1-10 μm
End.50g limestone powders are taken, addition is entered with the 5wt% dilute sulfuric acids of main composition-calcium carbonate equivalent in limestone powder or excess
Row 4 hours of reaction, generate calcium sulfate.After the calcium sulfate filtering that will be obtained, add water and be made into calcium sulphate soln and control its solution
Concentration be 10wt%, then add with lime stone weight ratio be 1:20 zinc sulfate is controlling temperature as catalyst
After 1 hour of hydro-thermal is carried out in 120 DEG C of autoclave, filtering is taken out, filtrate is semi-hydrated gypsum whisker, then semi-hydrated gypsum is brilliant
Dry 1 hour in 220 DEG C of drying oven must be immediately placed in, that is, obtains anhydrous gypsum whisker.
Embodiment 2
As shown in figure 1, after lime stone sludge is dried 3 hours at 500 DEG C, obtaining the agstone that particle diameter is for 1-10 μm
End.50g limestone powders are taken, addition is entered with the 15wt% dilute sulfuric acids of main composition-calcium carbonate equivalent in limestone powder or excess
Row 4 hours of reaction, generate calcium sulfate.After the calcium sulfate filtering that will be obtained, add water and be made into calcium sulphate soln and control its solution
Concentration be 10wt%, then add with lime stone weight ratio be 1:20 zinc sulfate is controlling temperature as catalyst
After 1 hour of hydro-thermal is carried out in 120 DEG C of autoclave, filtering is taken out, filtrate is semi-hydrated gypsum whisker, then semi-hydrated gypsum is brilliant
Dry 1 hour in 220 DEG C of drying oven must be immediately placed in, that is, obtains anhydrous gypsum whisker.
Embodiment 3
As shown in figure 1, after lime stone sludge is dried 2 hours at 650 DEG C, obtaining the agstone that particle diameter is for 1-10 μm
End.50g limestone powders are taken, addition is entered with the 15wt% dilute sulfuric acids of main composition-calcium carbonate equivalent in limestone powder or excess
Row 3 hours of reaction, generate calcium sulfate.After the calcium sulfate filtering that will be obtained, add water and be made into calcium sulphate soln and control its solution
Concentration be 30wt%, then add with lime stone weight ratio be 1:20 zinc sulfate is controlling temperature as catalyst
After 1.5 hours of hydro-thermal are carried out in 115 DEG C of autoclave, filtering is taken out, filtrate is semi-hydrated gypsum whisker, then by semi-hydrated gypsum
Whisker dries 1.5 hours in being immediately placed in 210 DEG C of drying oven, that is, obtain anhydrous gypsum whisker.
Embodiment 4
As shown in figure 1, after lime stone sludge is dried 4 hours at 450 DEG C, obtaining the agstone that particle diameter is for 1-10 μm
End.50g limestone powders are taken, addition is entered with the 5wt% dilute sulfuric acids of main composition-calcium carbonate equivalent in limestone powder or excess
Row 5 hours of reaction, generate calcium sulfate.After the calcium sulfate filtering that will be obtained, add water and be made into calcium sulphate soln and control its solution
Concentration be 20wt%, then add with lime stone weight ratio be 1:20 zinc sulfate is controlling temperature as catalyst
After 0.5 hour of hydro-thermal is carried out in 125 DEG C of autoclave, filtering is taken out, filtrate is semi-hydrated gypsum whisker, then by semi-hydrated gypsum
Whisker dries 0.5 hour in being immediately placed in 230 DEG C of drying oven, that is, obtain anhydrous gypsum whisker.
Embodiment 5
As shown in figure 1, after lime stone sludge is dried 3 hours at 500 DEG C, obtaining the agstone that particle diameter is for 1-10 μm
End.50g limestone powders are taken, the 7.5wt% dilute sulfuric acids with main composition-calcium carbonate equivalent or excess in limestone powder are added
Carry out reacting 4 hours, generate calcium sulfate.After the calcium sulfate filtering that will be obtained, add water and be made into calcium sulphate soln and control its molten
The concentration of liquid is 15wt%, and it is 1 then to add with lime stone weight ratio:20 zinc sulfate is warm in control as catalyst
After degree carries out 1 hour of hydro-thermal in 120 DEG C of autoclave, filtering is taken out, filtrate is semi-hydrated gypsum whisker, then by semi-hydrated gypsum
Whisker dries 1 hour in being immediately placed in 220 DEG C of drying oven, that is, obtain anhydrous gypsum whisker.
Embodiment 6
The anhydrous gypsum whisker that will be prepared in embodiment 1-5, is scanned using ESEM, as shown in Fig. 2 sweeping
Retouch Electronic Speculum SEM to amplify under conditions of 250 times, it can be observed that anhydrous gypsum whisker has filamentary structure.Meanwhile, using sweeping
The specification of the anhydrous gypsum whisker prepared in Electronic Speculum detection embodiment 1-5 is retouched, specific data are shown in Table 1.Can by table 1
Know, anhydrous gypsum whisker steady quality, the length of its whisker is about 100-180 μm, and draw ratio is about 60-100.It can be seen that, it is this
Filamentary structure, excellent performance can be widely applied to multiple fields.
The testing result of the material performance index of table 1.
| Classification | Whisker length value range (μm) | Whisker length (μm) | Draw ratio value range | Draw ratio |
| Embodiment 1 | 30-400 | 180 | 30-100 | 100 |
| Embodiment 2 | 30-400 | 180 | 30-100 | 100 |
| Embodiment 3 | 30-400 | 100 | 30-100 | 60 |
| Embodiment 4 | 30-400 | 100 | 30-100 | 60 |
| Embodiment 5 | 30-400 | 150 | 30-100 | 80 |
In sum, a kind of method for preparing crystal whisker of gypsum of the invention, is considered as useless using what is produced in steel industry
The lime stone sludge and sulfuric acid waste " turning waste into wealth " of slag, prepare the anhydrous gypsum whisker with excellent properties.The method is not
But the production cost of crystal whisker of gypsum is reduced, and protects environment, preferable shadow is produced with the harmonious development of environment to society
Ring.So, the present invention effectively overcomes various shortcoming of the prior art and has high industrial utilization.
The above-described embodiments merely illustrate the principles and effects of the present invention, not for the limitation present invention.It is any ripe
The personage for knowing this technology all can carry out modifications and changes under without prejudice to spirit and scope of the invention to above-described embodiment.Cause
This, those of ordinary skill in the art is complete with institute under technological thought without departing from disclosed spirit such as
Into all equivalent modifications or change, should be covered by claim of the invention.
Claims (2)
1. a kind of method for preparing crystal whisker of gypsum, comprises the steps of：
1) lime stone sludge is dried, obtains limestone powder；
2) addition dilute sulfuric acid reaction in a certain amount of limestone powder is taken, calcium sulfate is generated；
3) by step 2) in obtain calcium sulfate filtering after, add water and be made into calcium sulphate soln and control its concentration, add sulfuric acid
Used as catalyst, after carrying out hydro-thermal reaction, filtering obtains final product semi-hydrated gypsum whisker to zinc；
4) after semi-hydrated gypsum whisker is dried, anhydrous gypsum whisker is obtained；
Step 1) in, the drying temperature is 450-650 DEG C；The drying time is 2-4 hours；
Step 3) in, the zinc sulfate is 1 with the weight ratio of the addition of limestone powder:15-25；
Step 4) in, the condition of the dried process is：Treatment vessel：Drying oven；Treatment temperature：210-230℃；During treatment
Between：0.5-1.5 hours；
Step 1) in, the particle diameter of the limestone powder is 1-10 μm；
Step 2) in, the concentration of the dilute sulfuric acid is 5-15wt%；
Step 2) in, the reaction time is 3-5 hours；
Step 3) in, the concentration of the calcium sulphate soln is controlled to 10-30wt%；
Step 3) in, the condition of the hydro-thermal reaction is：Reaction vessel：Autoclave；Reaction temperature：115-125℃；During reaction
Between：0.5-1.5 hours.
2. application of a kind of lime stone sludge in crystal whisker of gypsum is prepared.
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