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CN106219565A - The preparation method of three hydrate zinc borates - Google Patents

The preparation method of three hydrate zinc borates Download PDF

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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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CN
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.)
Pending
Application number
CN201610590225.6A
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Chinese (zh)
Inventor
冯永成
刘茂海
何恒庆
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Zibo Wuwei Industrial Co Ltd
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Zibo Wuwei Industrial Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Zibo Wuwei Industrial Co Ltd filed Critical Zibo Wuwei Industrial Co Ltd
Priority to CN201610590225.6A priority Critical patent/CN106219565A/en
Publication of CN106219565A publication Critical patent/CN106219565A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B35/00Boron; Compounds thereof
    • C01B35/08Compounds containing boron and nitrogen, phosphorus, oxygen, sulfur, selenium or tellurium
    • C01B35/10Compounds containing boron and oxygen
    • C01B35/12Borates
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/61Micrometer sized, i.e. from 1-100 micrometer
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/11Powder tap density

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  • 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

The preparation method of three hydrate zinc borates
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.
CN201610590225.6A 2016-07-25 2016-07-25 The preparation method of three hydrate zinc borates Pending CN106219565A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
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Application Number Priority Date Filing Date Title
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Cited By (3)

* Cited by examiner, † Cited by third party
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)

* Cited by examiner, † Cited by third party
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

Patent Citations (3)

* Cited by examiner, † Cited by third party
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)

* Cited by examiner, † Cited by third party
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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Application publication date: 20161214

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