CN106219565A - The preparation method of three hydrate zinc borates - Google Patents
The preparation method of three hydrate zinc borates Download PDFInfo
- Publication number
- CN106219565A CN106219565A CN201610590225.6A CN201610590225A CN106219565A CN 106219565 A CN106219565 A CN 106219565A CN 201610590225 A CN201610590225 A CN 201610590225A CN 106219565 A CN106219565 A CN 106219565A
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- China
- Prior art keywords
- preparation
- boric acid
- hydrate
- hydrate zinc
- zinc oxide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- WGKLIJDVPACLGG-UHFFFAOYSA-N trizinc diborate hydrate Chemical class O.[Zn++].[Zn++].[Zn++].[O-]B([O-])[O-].[O-]B([O-])[O-] WGKLIJDVPACLGG-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000004327 boric acid Substances 0.000 claims abstract description 19
- 239000011787 zinc oxide Substances 0.000 claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- 239000010413 mother solution Substances 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000010792 warming Methods 0.000 claims abstract description 6
- 239000007787 solid Substances 0.000 claims abstract description 5
- 238000007664 blowing Methods 0.000 claims abstract description 3
- 239000000463 material Substances 0.000 claims description 6
- 235000021050 feed intake Nutrition 0.000 claims description 2
- 230000036632 reaction speed Effects 0.000 claims description 2
- 239000002994 raw material Substances 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052796 boron Inorganic materials 0.000 abstract description 4
- 238000000034 method Methods 0.000 abstract description 4
- 230000008878 coupling Effects 0.000 abstract description 3
- 238000010168 coupling process Methods 0.000 abstract description 3
- 238000005859 coupling reaction Methods 0.000 abstract description 3
- 239000002699 waste material Substances 0.000 abstract description 3
- 239000002351 wastewater Substances 0.000 abstract description 3
- IPCXNCATNBAPKW-UHFFFAOYSA-N zinc;hydrate Chemical compound O.[Zn] IPCXNCATNBAPKW-UHFFFAOYSA-N 0.000 abstract description 3
- 230000002349 favourable effect Effects 0.000 abstract description 2
- 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 description 8
- 239000003063 flame retardant Substances 0.000 description 7
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 239000012535 impurity Substances 0.000 description 6
- 229910052810 boron oxide Inorganic materials 0.000 description 5
- 238000001354 calcination Methods 0.000 description 5
- 238000002425 crystallisation Methods 0.000 description 4
- 230000008025 crystallization Effects 0.000 description 4
- 230000004044 response Effects 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000002352 surface water Substances 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 229920001971 elastomer Polymers 0.000 description 2
- 230000001629 suppression Effects 0.000 description 2
- 229920002725 thermoplastic elastomer Polymers 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- 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 1
- 229910011255 B2O3 Inorganic materials 0.000 description 1
- 241001597008 Nomeidae Species 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 229910021538 borax Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 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
- 239000013078 crystal Substances 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 210000003739 neck Anatomy 0.000 description 1
- 150000002896 organic halogen compounds Chemical class 0.000 description 1
- 239000000075 oxide glass Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 230000011514 reflex Effects 0.000 description 1
- 230000011218 segmentation Effects 0.000 description 1
- 239000004328 sodium tetraborate Substances 0.000 description 1
- 235000010339 sodium tetraborate Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/11—Powder tap density
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Fireproofing Substances (AREA)
Abstract
The present invention relates to the preparation method of a kind of three hydrate zinc borates, first add water, be subsequently adding boric acid and be warming up to 40 60 DEG C, it is subsequently adding zinc oxide, is warming up to 75 95 DEG C, react blowing after 6 10h, add water rinsing 15 45 minutes, enters centrifuge through secondary filter, and solid drying obtains three hydrate zinc borates.Present invention process is simple, yield height, low cost, produces without the three wastes, and reaction raw materials has only to boric acid, zinc oxide and water, reaction condition gentleness, no coupling product and waste water generation, and mother solution can recycle, and there is not the loss of boron.The big production cost in workshop is low, and product quality is high, obtains the consistent favorable comment of client in association area.
Description
Technical field
The present invention relates to the preparation method of a kind of three hydrate zinc borates.
Background technology
Fire retardant Firebrake ZB is that United States Borax Inc. develops, and Firebrake ZB is a kind of multifunctional fire retardant, and structural formula is
XZnO YB2O3ZH2O, that the most extensive consumption of purposes is maximum is 2ZnO 3B2O33.5H2O, the most also 2ZnO 3B2O37H2O、
2ZnO 2B2O33H2O, 2ZnO 3B2O3, 3ZnO 2B2O35H2The multiple derivant such as O.
Firebrake ZB is white crystals fine-powder, water insoluble, is slightly soluble in hot water and is soluble in strong acid.Firebrake ZB is mainly used
Make fire retardant, antismoke agent, antibacterial etc., in engineering plastics to be applied to, rubber, cable, coating, pottery, glass, timber, doctor
The industries such as treatment.The fire retardant mechanism of Firebrake ZB divides three aspects: absorb heat and diluting effect, covering effect and suppression chain reaction.Boric acid
Zinc is heated to uniform temperature, i.e. releases water of crystallization, absorbs a large amount of heat energy, reduces combustion front temperature, and the moisture discharged can be dilute
Releasing the oxygen in air, suppression burning occurs, and generates boric oxide glass shape thin film simultaneously, covers and play heat insulation resistance oxygen on polymer
Effect.Firebrake ZB compounds with organohalogen compounds, and during burning, generation ZnX and boric acid overlay are in comburant surface, every
Absolutely air, and the HX that BX3 releases when burning is to stoping the chain reflex between high mars free radical to have catalytic action, from
And reach flame retardant effect more more preferable than alone Firebrake ZB.
3.5 hydrate zinc borates are the models that most widely used general consumption is maximum, 3.5 hydrate zinc borate advantages: good flame retardation effect, heat are steady
Qualitative height, dehydration temperature are high, just lose water of crystallization more than 300 DEG C.Along with Firebrake ZB is in the extensive application of every profession and trade, now towards
The direction of segmentation is developed.The fire retardant needed in some field need not reach more than 300 DEG C and just loses water of crystallization, needs relatively low
At a temperature of (200 DEG C) just can lose water of crystallization and play fire-retardant effect, and three hydrate zinc borates are because of its relatively low dehydration temperature very
Good meets needs, and three hydrate zinc borates are widely used in the necks such as papermaking, polyurethane, thermoplastic elastomer (TPE), polyolefin, rubber, PVC
Territory.
Three hydrate zinc borate overwhelming majority poor quality of market production and sales, impurity is many, and main content boron oxide content is on the low side, oxygen
Changing Zn content higher, calcination loss is on the low side, and mobility is bad, and impurity stain is many.The present invention throws by adjusting boric acid and zinc oxide
Material ratio, reaction temperature, in the range of not only making main content boron oxide, zinc oxide accomplish standard index, and calcination loss also reaches
More than 14, the production response time also shortens dramatically, and improves the utilization rate of still;Rinse through potcher, make product proportion become big
Mobility improves;Through secondary filter, well control impurity and stain.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of three hydrate zinc borates, technique is simple, yield height, low cost,
Producing without the three wastes, reaction raw materials has only to boric acid, zinc oxide and water, and reaction condition is gentle, and no coupling product and waste water produce, mother solution
Can recycle, there is not the loss of boron.The big production cost in workshop is low, and product quality is high.
The preparation method of a kind of three hydrate zinc borates of the present invention, first adds water, is subsequently adding boric acid and is warming up to 40-60
DEG C, it being subsequently adding zinc oxide, be warming up to 75-95 DEG C, blowing after reaction 6-10h, add water rinsing 15-45 minute, through accurate mistake
Filter enters centrifuge, and solid drying obtains three hydrate zinc borates.
Reaction speed of agitator controls at 60-80r/min.
The mother solution that centrifuge produces returns to reactor and recycles.
The mass ratio of water and boric acid is at 3-5:1.
The feed intake ratio of amount of material of boric acid and zinc oxide is 2.0-2.1:1.
The chemical formula 2ZnO 2B of three hydrate zinc borates of the present invention2O33H2O。
The present invention three hydrate zinc borate Testing index such as table 1:
Table 1 three hydrate zinc borate Testing index
| Raw material composition and detection performance | Testing result |
| Boron oxide, % | 37.5-40.0 |
| Zinc oxide, % | 44.0-47.0 |
| Calcination loss, % | 13.5-14.5 |
| Surface water, %≤ | 0.5 |
| Middle particle diameter, um | 5-8 |
| Whiteness, >= | 98 |
| Bulk density, kg/m3 | 560-650 |
| Impurity, %≤ | 0.1 |
Compared with prior art, the method have the advantages that
The preparation method of the present invention, technique is simple, yield height, low cost, without three wastes generation, reaction raw materials has only to boron
Acid, zinc oxide and water, reaction condition is gentle, and no coupling product and waste water produce, and mother solution can recycle, and there is not the loss of boron.
The big production cost in workshop is low, and product quality is high, obtains the consistent favorable comment of client in association area.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described further.
Embodiment 1
In 3 tons of reactors, adding 1600-2500 kg of water, add 572 kilograms of boric acid, temperature rises to 60 DEG C, adds 375 kilograms
Zinc oxide, boric acid is 2:1 with the ratio of the amount of zinc oxide materials, 10 hours response time, temperature 75 DEG C, rotating speed 60-80r/min,
React complete being discharged in potcher, add isopyknic water and rinse half an hour, after secondary filter, enter centrifuge, solid warp
Drying machine drying obtains target product 780 kilograms, and the mother solution that centrifuge produces returns to reactor and recycles.
Product checking result such as table 2.
Table 2 Product checking result
| Raw material composition and detection performance | Testing result |
| Boron oxide, % | 37.89 |
| Zinc oxide, % | 47.06 |
| Calcination loss, % | 13.91 |
| Surface water, %≤ | 0.35 |
| Middle particle diameter, um | 6.03 |
| Whiteness, >= | 98 |
| Bulk density, kg/m3 | 594 |
| Impurity, %≤ | 0.08 |
Embodiment 2
In 3 tons of reactors, adding 1600-2500 kg of water, add 586 kilograms of boric acid, temperature rises to 60 DEG C, adds 375 kilograms
Zinc oxide, boric acid is 2.05:1 with the ratio of the amount of zinc oxide materials, 8 hours response time, temperature 85 DEG C, rotating speed 60-80r/
Min, reacts complete and is discharged in potcher, adds isopyknic water and rinses half an hour, enters centrifuge after secondary filter, Gu
Body drying machine is dried and is obtained target product 791 kilograms, and the mother solution that centrifuge produces returns to reactor and recycles.
Product checking result such as table 3.
Table 3 Product checking result
| Raw material composition and detection performance | Testing result |
| Boron oxide, % | 38.44 |
| Zinc oxide, % | 46.03 |
| Calcination loss, % | 14.08 |
| Surface water, %≤ | 0.37 |
| Middle particle diameter, um | 5.89 |
| Whiteness, >= | 98 |
| Bulk density, kg/m3 | 604 |
| Impurity, %≤ | 0.08 |
Embodiment 3
In 3 tons of reactors, adding 1600-2500 kg of water, add 600 kilograms of boric acid, temperature rises to 60 DEG C, to boric acid almost
Being completely dissolved, add 375 kilograms of zinc oxide, boric acid is 2.1:1 with the ratio of the amount of zinc oxide materials, 6.5 hours response time, temperature
95 DEG C, rotating speed 60-80r/min, reacts complete and is discharged in potcher, add isopyknic water and rinse half an hour, through accurate mistake
Entering centrifuge after filter, solid drying machine is dried and is obtained target product 823 kilograms, and the mother solution that centrifuge produces returns to reactor
Recycle.
Product checking result such as table 4.
Table 4 Product checking result
Claims (5)
1. the preparation method of a hydrate zinc borate, it is characterised in that first add water, is subsequently adding boric acid and is warming up to 40-60 DEG C, so
Rear addition zinc oxide, is warming up to 75-95 DEG C, blowing after reaction 6-10h, and add water rinsing 15-45 minute, enters through secondary filter
Centrifuge, solid drying obtains three hydrate zinc borates.
The preparation method of three hydrate zinc borates the most according to claim 1, it is characterised in that reaction speed of agitator controls
60-80r/min。
The preparation method of three hydrate zinc borates the most according to claim 1, it is characterised in that the mother solution that centrifuge produces returns to
Reactor recycles.
The preparation method of three hydrate zinc borates the most according to claim 1, it is characterised in that the mass ratio of water and boric acid is at 3-
5:1。
The preparation method of three hydrate zinc borates the most according to claim 1, it is characterised in that boric acid and zinc oxide feed intake material
The ratio of amount be 2.0-2.1:1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610590225.6A CN106219565A (en) | 2016-07-25 | 2016-07-25 | The preparation method of three hydrate zinc borates |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610590225.6A CN106219565A (en) | 2016-07-25 | 2016-07-25 | The preparation method of three hydrate zinc borates |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106219565A true CN106219565A (en) | 2016-12-14 |
Family
ID=57532376
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610590225.6A Pending CN106219565A (en) | 2016-07-25 | 2016-07-25 | The preparation method of three hydrate zinc borates |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106219565A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107235496A (en) * | 2017-07-07 | 2017-10-10 | 辽宁大学 | A kind of Firebrake ZB ZnB2O4The low temperature preparation method of luminescent material |
| CN107381590A (en) * | 2017-07-27 | 2017-11-24 | 山东五维阻燃科技股份有限公司 | The preparation method of low chloroboric acid zinc |
| CN115286006A (en) * | 2022-08-31 | 2022-11-04 | 山东五维阻燃科技股份有限公司 | Preparation method of high-temperature-resistant anhydrous zinc borate |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1603237A (en) * | 2004-09-30 | 2005-04-06 | 武汉大学 | The preparation method of zinc borate |
| CN1789135A (en) * | 2005-12-12 | 2006-06-21 | 中国科学院青海盐湖研究所 | Hydrothermal method for preparation of shape-controllable low-hydrate zinc borate powder |
| 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 |
-
2016
- 2016-07-25 CN CN201610590225.6A patent/CN106219565A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1603237A (en) * | 2004-09-30 | 2005-04-06 | 武汉大学 | The preparation method of zinc borate |
| CN1789135A (en) * | 2005-12-12 | 2006-06-21 | 中国科学院青海盐湖研究所 | Hydrothermal method for preparation of shape-controllable low-hydrate zinc borate powder |
| 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 |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107235496A (en) * | 2017-07-07 | 2017-10-10 | 辽宁大学 | A kind of Firebrake ZB ZnB2O4The low temperature preparation method of luminescent material |
| CN107381590A (en) * | 2017-07-27 | 2017-11-24 | 山东五维阻燃科技股份有限公司 | The preparation method of low chloroboric acid zinc |
| CN107381590B (en) * | 2017-07-27 | 2019-08-30 | 山东五维阻燃科技股份有限公司 | The preparation method of low chlorine borate zinc |
| CN115286006A (en) * | 2022-08-31 | 2022-11-04 | 山东五维阻燃科技股份有限公司 | Preparation method of high-temperature-resistant anhydrous zinc borate |
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