CN108706606A - A kind of process preparing zinc borate - Google Patents
A kind of process preparing zinc borate Download PDFInfo
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- CN108706606A CN108706606A CN201810933037.8A CN201810933037A CN108706606A CN 108706606 A CN108706606 A CN 108706606A CN 201810933037 A CN201810933037 A CN 201810933037A CN 108706606 A CN108706606 A CN 108706606A
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- zinc
- zinc borate
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- process preparing
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- BIKXLKXABVUSMH-UHFFFAOYSA-N trizinc;diborate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]B([O-])[O-].[O-]B([O-])[O-] BIKXLKXABVUSMH-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 36
- 238000006243 chemical reaction Methods 0.000 claims abstract description 45
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 42
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000013078 crystal Substances 0.000 claims abstract description 24
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims abstract description 21
- 229960001763 zinc sulfate Drugs 0.000 claims abstract description 21
- 229910000368 zinc sulfate Inorganic materials 0.000 claims abstract description 21
- 239000007788 liquid Substances 0.000 claims abstract description 18
- 239000007787 solid Substances 0.000 claims abstract description 17
- 229910021538 borax Inorganic materials 0.000 claims abstract description 16
- 238000002425 crystallisation Methods 0.000 claims abstract description 16
- 230000008025 crystallization Effects 0.000 claims abstract description 16
- 239000004328 sodium tetraborate Substances 0.000 claims abstract description 16
- 235000010339 sodium tetraborate Nutrition 0.000 claims abstract description 16
- 239000011787 zinc oxide Substances 0.000 claims abstract description 15
- WQSRXNAKUYIVET-UHFFFAOYSA-N sulfuric acid;zinc Chemical compound [Zn].OS(O)(=O)=O WQSRXNAKUYIVET-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000012216 screening Methods 0.000 claims abstract description 6
- 239000012467 final product Substances 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 238000004321 preservation Methods 0.000 claims description 13
- 238000001816 cooling Methods 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 5
- OMUGFZNEOIWQOD-UHFFFAOYSA-N boric acid;zinc Chemical compound [Zn].OB(O)O OMUGFZNEOIWQOD-UHFFFAOYSA-N 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 3
- 238000012805 post-processing Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 2
- 238000000967 suction filtration Methods 0.000 claims 1
- 239000000047 product Substances 0.000 abstract description 45
- 230000018044 dehydration Effects 0.000 abstract description 12
- 238000006297 dehydration reaction Methods 0.000 abstract description 12
- 239000002245 particle Substances 0.000 abstract description 6
- 239000002994 raw material Substances 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 10
- 230000000694 effects Effects 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 238000009413 insulation Methods 0.000 description 5
- 239000000376 reactant Substances 0.000 description 5
- 230000007547 defect Effects 0.000 description 4
- 239000003063 flame retardant Substances 0.000 description 4
- 238000009826 distribution Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- 230000001629 suppression Effects 0.000 description 2
- 229940007718 zinc hydroxide Drugs 0.000 description 2
- 229910021511 zinc hydroxide Inorganic materials 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000012876 carrier material Substances 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 235000019504 cigarettes Nutrition 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- RSCACTKJFSTWPV-UHFFFAOYSA-N disodium;3,7-dioxido-2,4,6,8,9-pentaoxa-1,3,5,7-tetraborabicyclo[3.3.1]nonane;pentahydrate Chemical compound O.O.O.O.O.[Na+].[Na+].O1B([O-])OB2OB([O-])OB1O2 RSCACTKJFSTWPV-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000004079 fireproofing Methods 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 230000009916 joint effect Effects 0.000 description 1
- 231100001231 less toxic Toxicity 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000032696 parturition Effects 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 238000012430 stability testing Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000002411 thermogravimetry Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- UGZADUVQMDAIAO-UHFFFAOYSA-L zinc hydroxide Chemical compound [OH-].[OH-].[Zn+2] UGZADUVQMDAIAO-UHFFFAOYSA-L 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B35/00—Boron; Compounds thereof
- C01B35/08—Compounds containing boron and nitrogen, phosphorus, oxygen, sulfur, selenium or tellurium
- C01B35/10—Compounds containing boron and oxygen
- C01B35/12—Borates
- C01B35/127—Borates of heavy metals
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/88—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by thermal analysis data, e.g. TGA, DTA, DSC
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
Abstract
The invention discloses a kind of processes preparing zinc borate, first water is added to be configured to solution of zinc sulfate on solid sulphuric acid zinc, and solution of zinc sulfate is adjusted to pH=2~4, borax, zinc oxide, zinc borate crystal seed and water is then added so that solid-liquid mass ratio is 1~1.5：1, heating reaction adds the water with quality such as solids, cools down, keeps the temperature crystallization, post-process to obtain the final product.The present invention prepares zinc borate using borax, solution of zinc sulfate and zinc oxide as primary raw material, by adjusting pH value in reaction, the methods of control reaction solid-to-liquid ratio increases substantially product quality, crystal seed by the way that the particular particle size range by screening is added guides zinc borate crystal growing process, prepares the product of size uniformity.The good heat stability of gained zinc borate of the invention, 1% dehydration temperaturre are up to 345 DEG C.
Description
Technical field
The present invention relates to a kind of processes preparing zinc borate.Belong to chemosynthesis technical field.
Background technology
Zinc borate is earliest one of inorganic combustion inhibitor, be one kind have it is fire-retardant, glow at charcoal, suppression cigarette, suppression and prevent from giving birth to
At the multifunction additive of a variety of efficiency such as molten drop, and with the characteristics such as less toxic, inexpensive, transparency is high and is not easy to precipitate.Cause
For zinc borate 2ZnO3B2O3·3.5H2O has higher dehydration temperaturre, the crystallization water is still retained at 250 DEG C or more, therefore have
There is higher commercial value.But zinc borate industrial manufacturing process traditional at present limits its product there are a large amount of defect
Application and popularization.Such as：Boric acid-zinc hydroxide method, required zinc hydroxide needs are prepared in situ, and complex process and can not keep away
Generate a large amount of by-products and waste water with exempting from.Borax-zincate process, preparation process is by a relatively simple, but preparation domestic at present
Technique is excessively coarse, causes product quality deficient, and thermal stability is poor, and 1% dehydration temperaturre is generally less than 320 DEG C, with the U.S.
330 DEG C of 1% dehydration temperaturre of imported product U.S. boron greatly differs from each other.
Inorganic anti-flaming material is used as additive application in engineering material such as plastics, rubber, coating, fabrics more, is promoted
The flame retardant effect of material, therefore the microscopic dimensions of fire proofing itself and pattern are to its carrier material self performance and difficult processing
Degree has significant impact.The inorganic material that Size Distribution is uniform, pattern is regular can reduce the difficulty of processing of engineering material, show
More stable flame retardant property, it is not easy to destroy the primary characteristic of engineering material itself.But zinc borate domestic at present is fire-retardant
The universal particle diameter distribution of product is wider, and pattern is irregular, this brings many obstacles to the following process of product and application.
In conclusion for the preparation process of domestic zinc borate products, presently, there are problems with：(1) technique falls behind, instead
Answer condition unreasonable, product quality is low, and especially thermal stability is poor；(2) product size distributing inhomogeneity, pattern are not advised
Then, following process difficulty is big, performance is less than imported product.
Invention content
The purpose of the present invention is to overcome above-mentioned the deficiencies in the prior art, provide a kind of process preparing zinc borate.
To achieve the above object, the present invention uses following technical proposals：
Solid sulphuric acid zinc is first added water to be configured to solution of zinc sulfate by a kind of process preparing zinc borate, and by sulfuric acid
Zinc solution is adjusted to pH=2~4, and borax, zinc oxide, zinc borate crystal seed and water is then added so that and solid-liquid mass ratio is 1~
1.5：1, heating reaction adds the water with quality such as solids, cools down, keeps the temperature crystallization, post-process to obtain the final product.
Preferably, the process is as follows：
(1) solid sulphuric acid zinc adds water to prepare solution of zinc sulfate, adjusts pH=2~4, is added in reaction kettle；
(2) borax, zinc oxide, zinc borate crystal seed and water is added so that solid-liquid mass ratio is 1~1.5：1；
(3) 95~102 DEG C are heated to react 4~6 hours, is subsequently added into the water with quality such as solids；
(4) 50 DEG C are naturally cooling to, heat preservation crystallization 2~4 hours post-processes to obtain the final product.
Preferably, the pH value that solution of zinc sulfate is adjusted by the way that the concentrated sulfuric acid is added dropwise, can determine sulphur according to the quality requirements of product
The pH value of sour zinc solution adjusts terminal.
Preferably, the zinc borate crystal seed is the boric acid zinc powder by screening.
It is further preferred that the zinc borate crystal seed be by metallic screen isolate size be 1~5 μm, 6~10 μm or
11~20 μm of zinc borate, effect is that different product sizes and pattern may be guided out.
Preferably, the mass fraction of the solution of zinc sulfate is 35%.
Preferably, the mass ratio of solid sulphuric acid zinc, borax, zinc oxide and zinc borate crystal is 40~50：60~70：0.1
~0.5：0.02~0.05.
Preferably, the temperature of the heating reaction is 95~102 DEG C, and the reaction time is 4~6 hours.
Preferably, the cooling is Temperature fall.
Preferably, the temperature of the heat preservation crystallization is 50 DEG C, and heat preservation crystallization time is 2~4 hours.
Preferably, the post-processing includes filtering, wash and drying.
Beneficial effects of the present invention：
The present invention prepares zinc borate using borax, solution of zinc sulfate and zinc oxide as primary raw material, by adjusting pH value in reaction,
The methods of control reaction solid-to-liquid ratio increases substantially product quality, and the crystal seed by the way that the particular particle size range by screening is added draws
Zinc borate crystal growing process is led, the product of size uniformity is prepared.The good heat stability of gained zinc borate of the invention, 1%
Dehydration temperaturre is up to 345 DEG C.
The present invention is carried out to guide to react to control by adjusting pH value, reaction temperature and solid-liquid ratio in reaction system
Product form processed, pH value and temperature in system adjust the reactivity of zinc ion and borax jointly, and solid-to-liquid ratio decides
The ratio of water in the viscosity and product form of reaction system, the above influence factor synergistic effect, joint effect product most
Composition and quality eventually.The present invention is 2ZnO by regulating and controlling the method for pH value of solution and system solid-to-liquid ratio to realize product form
3B2O3·3.5H2The effect of O, solves the unstable defect of traditional product quality, and thermogravimetric analysis shows to meet state in water content
Under the premise of family's standard, 1% dehydration temperaturre is high, is better than imported product performance.
Since the grain size and pattern of product can influence subsequent processing using effect, found by multigroup contrast experiment
This influence factor and the size of crystal seed used in reaction process have consistent relationship, the present invention further to be led to according to result of study
Crystal seed of the zinc borate products within the scope of screening specified particle diameter as reaction is crossed, to guide reaction product to fixed dimension and pattern
Growth, to realize product grain size, pattern homogenization, further promoted product machinability and using effect, solve
The applied defect of traditional handicraft product.
Description of the drawings
Fig. 1 is that 1 product of embodiment and the thermogravimetric curve of comparative example product compare；
Fig. 2 a are the electron-microscope scanning figure of 1 product of embodiment；
Fig. 2 b are the electron-microscope scanning figure of comparative example product.
Specific implementation mode
The present invention will be further elaborated with reference to the accompanying drawings and examples, it should which explanation, following the description is only
It is not to be defined to its content to explain the present invention.
Embodiment 1：
Add water 83.5g to be configured to the solution that content mass fraction is 35% in the zinc sulfate of 45g, adjusts the pH value of its solution
It is 3, is added into reaction kettle, by the borax (borax pentahydrate) of 67g, 1-5 μm of zinc borate of the zinc oxide of 0.3g, 0.03g
Crystal seed is added reaction kettle and adds 2.9g water according to the ratio of the solid reactant and water that are added above, and it is 1.3 to make system solid-to-liquid ratio：
1, it starts to warm up to 97 DEG C and reacts, insulation reaction is after 5 hours, to reaction kettle plus waits the water of 112.33g, is naturally cooling to 50 DEG C,
Heat preservation crystallization is reacted after 3 hours to be terminated.Reaction solution is filtered, is washed, can be obtained product of the present invention after 80 DEG C of drying 2h.
Embodiment 2：
Water 74.3g is added to be configured to the solution that content is 35% in the zinc sulfate of 40g, the pH value for adjusting its solution is 2, by it
It is added in reaction kettle, reaction kettle is added in the 6-10 μm of zinc borate crystal seed of the borax of 70g, the zinc oxide of 0.5g, 0.02g, according to
The ratio of the solid reactant and water that are added above adds the water of 34.72g that system solid-to-liquid ratio is made to be 1.5：1, it starts to warm up to 95 DEG C
Reaction, insulation reaction, to reaction kettle plus the water of 110.52g, are naturally cooling to 50 DEG C, heat preservation crystallization is reacted after 2 hours after 6 hours
Terminate.Reaction solution is filtered, is washed, can be obtained product of the present invention after 80 DEG C of drying 2h.
Embodiment 3：
By the zinc sulfate of 50g add water 93g be configured to content be 35% solution, adjust its solution pH value be 4, by itself plus
Enter in reaction kettle, reaction kettle is added in the zinc borate crystal seed of the borax of 60g, the zinc oxide of 0.1g, 0.05g, is added according to above
Solid reactant and water ratio, add 17.05g water make system solid-to-liquid ratio be 1：1, it starts to warm up to 102 DEG C and reacts, heat preservation is anti-
After answering 4 hours, to reaction kettle plus 110.15g water is waited, is naturally cooling to 50 DEG C, heat preservation crystallization is reacted after 4 hours to be terminated.It will reaction
Liquid is filtered, washing, can be obtained product of the present invention after 80 DEG C of drying 2h.
Embodiment 4：
Water 78g is added to be configured to the solution that content is 35% in the zinc sulfate of 42g, the pH value for adjusting its solution is 2.5, by it
It is added in reaction kettle, reaction kettle, root is added in 11-20 μm of the zinc borate crystal seed of the borax of 68g, the zinc oxide of 0.4g, 0.04g
The ratio of the upper solid reactant and water being added according to this adds 7g water that system solid-to-liquid ratio is made to be 1.3：1, it starts to warm up to 99 DEG C instead
It answers, insulation reaction, to reaction kettle plus 110.44g water, is naturally cooling to 50 DEG C, heat preservation crystallization reacts knot after 3 hours after 5 hours
Beam.Reaction solution is filtered, is washed, 80 DEG C of drying 2h, you can obtain product of the present invention.
Embodiment 5：
Water 87g is added to be configured to the solution that content is 35% in the zinc sulfate of 47g, the pH value for adjusting its solution is 3.5, by it
It is added in reaction kettle, reaction kettle is added in 6~10 μm of zinc borate crystal seeds of the borax of 62g, the zinc oxide of 0.2g, 0.02g, according to
The ratio of the solid reactant and water that are added above adds 3g water that system solid-to-liquid ratio is made to be 1.2：1, it starts to warm up to 96 DEG C and reacts,
After insulation reaction 5 hours, to reaction kettle plus 109.22g water is waited, is naturally cooling to 50 DEG C, heat preservation crystallization is reacted after 3 hours to be terminated.
Reaction solution is filtered, is washed, 80 DEG C of drying 2h, you can obtain product of the present invention.
Comparative example
Add water 83.6g to be configured to the solution that content is 35% in the zinc sulfate of 45g, is added into reaction kettle, by 67g's
Borax, the zinc oxide of 0.3g, 0.03g common boric acid zinc powder (;20 μm) reaction kettle is added, it is anti-according to the solid being added above
The ratio for answering object and water adds 2.8g water that system solid-to-liquid ratio is made to be 1.3：1, it starts to warm up to 97 DEG C and reacts, insulation reaction 5 hours
Afterwards, to reaction kettle plus 112.33g water is waited, is naturally cooling to 50 DEG C, heat preservation crystallization is reacted after 3 hours to be terminated.Reaction solution is carried out
It filters, washing, 80 DEG C of drying 2h, you can obtain comparative example product.
Test example
1, product heat stability testing：Hot mistake is carried out to the product zinc borate of representative embodiment 1 and comparative example
Weight analysis, test result are shown in Table 1 and Fig. 1.
1. embodiment 1 of table and comparative example product thermal weight loss data
| 0.5% dehydration temperaturre/DEG C | 1% dehydration temperaturre/DEG C | 1.5% dehydration temperaturre/DEG C | |
| Embodiment 1 | 315.36 | 345.95 | 359.58 |
| Comparative example | 272.53 | 317.49 | 341.72 |
Conclusion：Comparative example does not carry out pH value adjustment to solution of zinc sulfate, and used zinc borate crystal seed is common zinc borate
Powder, 0.5% dehydration temperaturre, 1% dehydration temperaturre and 1.5% dehydration temperaturre well below embodiment 1, embodiment 1
Thermal stability is more preferably.
2, product size, pattern：Electron-microscope scanning is carried out to the product zinc borate of representative embodiment 1 and comparative example
Characterization, test result are shown in Fig. 2 a and Fig. 2 b.
Conclusion：Electron-microscope scanning figure 2b shown in comparative example shows that the zinc borate not plus obtained by the zinc borate crystal seed through screening is general
Wider all over particle diameter distribution, pattern is irregular；The representative 1 gained zinc borate products electron microscope 2a of embodiment of the application is aobvious
To show, product crystal form crystalline substance looks are preferable, uniform particle diameter, are applied to engineering material and show that the machinability of product and using effect are preferable,
Solves the applied defect of traditional handicraft product.
Above-mentioned, although the foregoing specific embodiments of the present invention is described with reference to the accompanying drawings, not protects model to the present invention
The limitation enclosed, based on the technical solutions of the present invention, those skilled in the art, which need not make the creative labor, to be done
The various modifications or changes gone out are still within protection scope of the present invention.
Claims (10)
1. a kind of process preparing zinc borate, which is characterized in that first add water to be configured to solution of zinc sulfate on solid sulphuric acid zinc,
And solution of zinc sulfate is adjusted to pH=2~4, borax, zinc oxide, zinc borate crystal seed and water is then added so that solid-liquid matter
Amount is than being 1~1.5：1, heating reaction adds the water with quality such as solids, cools down, keeps the temperature crystallization, post-process to obtain the final product.
2. a kind of process preparing zinc borate according to claim 1, which is characterized in that the tool of the process
Steps are as follows for body：
(1) solid sulphuric acid zinc adds water to prepare solution of zinc sulfate, adjusts pH=2~4, is added in reaction kettle；
(2) borax, zinc oxide, zinc borate crystal seed and water is added so that solid-liquid mass ratio is 1~1.5：1；
(3) 95~102 DEG C are heated to react 4~6 hours, is subsequently added into the water with quality such as solids；
(4) 50 DEG C are naturally cooling to, heat preservation crystallization 2~4 hours post-processes to obtain the final product.
3. a kind of process preparing zinc borate according to claim 1 or 2, which is characterized in that the zinc sulfate is molten
The adjusting method of liquid pH value is：The concentrated sulfuric acid is added dropwise and adjusts pH.
4. a kind of process preparing zinc borate according to claim 1 or 2, which is characterized in that the zinc borate is brilliant
Kind is the boric acid zinc powder by screening.
5. a kind of process preparing zinc borate according to claim 4, which is characterized in that the zinc borate crystal seed is
By metallic screen isolate size be 1~5 μm, 6~10 μm, 11~20 μm of boric acid zinc powder.
6. a kind of process preparing zinc borate according to claim 1 or 2, which is characterized in that the zinc sulfate is molten
The mass fraction of liquid is 35%.
7. a kind of process preparing zinc borate according to claim 1 or 2, which is characterized in that zinc sulfate, borax,
The mass ratio of zinc oxide and zinc borate crystal seed is 40~50：60~70：0.1~0.5：0.02~0.05.
8. a kind of process preparing zinc borate according to claim 1, which is characterized in that the temperature for heating reaction is
95~102 DEG C, the reaction time is 4~6 hours.
9. a kind of process preparing zinc borate according to claim 1, which is characterized in that the temperature of the heat preservation crystallization
Degree is 50 DEG C, and heat preservation crystallization time is 2~4 hours.
10. a kind of process preparing zinc borate according to claim 1 or 2, which is characterized in that the post-processing packet
Include suction filtration, washing and drying.
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| CN201810933037.8A CN108706606A (en) | 2018-08-16 | 2018-08-16 | A kind of process preparing zinc borate |
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| CN201810933037.8A CN108706606A (en) | 2018-08-16 | 2018-08-16 | A kind of process preparing zinc borate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109970074A (en) * | 2018-10-25 | 2019-07-05 | 青岛科技大学 | A kind of preparation method of the zinc borate of high thermal stability |
| CN112147188A (en) * | 2020-09-24 | 2020-12-29 | 青岛科技大学 | Method for rapidly determining ash content in vulcanization accelerator MBTS |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5472644A (en) * | 1991-11-22 | 1995-12-05 | U.S. Borax Inc. | Zinc borate |
| CN101704532A (en) * | 2009-11-10 | 2010-05-12 | 武汉大学 | Preparation method of zinc borate |
| CN102267702A (en) * | 2011-07-04 | 2011-12-07 | 北京石油化工学院 | Method for preparing sub-micron zinc borate by virtue of alcohol-water method |
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| CN105504346A (en) * | 2015-12-16 | 2016-04-20 | 安徽壹石通材料科技股份有限公司 | Preparation method of novel zinc borate flame-retardant material |
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| CN109970074A (en) * | 2018-10-25 | 2019-07-05 | 青岛科技大学 | A kind of preparation method of the zinc borate of high thermal stability |
| CN112147188A (en) * | 2020-09-24 | 2020-12-29 | 青岛科技大学 | Method for rapidly determining ash content in vulcanization accelerator MBTS |
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Inventor after: Feng Weichun Inventor after: Yue Tao Inventor after: Liu Qikui Inventor after: Gao Weidan Inventor after: Zhai Yunge Inventor after: Wang Ruifei Inventor after: Xing Wenguo Inventor before: Yue Tao Inventor before: Xing Wenguo Inventor before: Feng Weichun Inventor before: Gao Weidan Inventor before: Zhai Yunge Inventor before: Wang Ruifei |
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Application publication date: 20181026 |