[go: up one dir, main page]

CN104150502A - Method for preparing zinc borate crystals by using zinc borate whisker mother liquor - Google Patents

Method for preparing zinc borate crystals by using zinc borate whisker mother liquor Download PDF

Info

Publication number
CN104150502A
CN104150502A CN201410384292.3A CN201410384292A CN104150502A CN 104150502 A CN104150502 A CN 104150502A CN 201410384292 A CN201410384292 A CN 201410384292A CN 104150502 A CN104150502 A CN 104150502A
Authority
CN
China
Prior art keywords
zinc borate
mother liquor
crystal
crystals
preparation
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.)
Granted
Application number
CN201410384292.3A
Other languages
Chinese (zh)
Other versions
CN104150502B (en
Inventor
刘鑫
边绍菊
高丹丹
朱东海
党力
景燕伟
董亚萍
李武
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Qinghai Institute of Salt Lakes Research of CAS
Original Assignee
Qinghai Institute of Salt Lakes Research of CAS
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 Qinghai Institute of Salt Lakes Research of CAS filed Critical Qinghai Institute of Salt Lakes Research of CAS
Priority to CN201410384292.3A priority Critical patent/CN104150502B/en
Publication of CN104150502A publication Critical patent/CN104150502A/en
Application granted granted Critical
Publication of CN104150502B publication Critical patent/CN104150502B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Landscapes

  • Crystals, And After-Treatments Of Crystals (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

The invention relates to a method for preparing zinc borate crystals by using zinc borate whisker mother liquor. The zinc borate whisker mother liquor is used for preparing Zn3B10O18.14H2O crystals by the following steps: adding water into the zinc borate whisker mother liquor to form a mixed solution, wherein the amount of the water is 1 to 40 percent of the weight of the zinc borate whisker mother liquor; reacting the mixed solution for 1 to 24 h in a water bath of 20 to 90 DEG C; standing the reacted mixed solution for 7 to 14 days; filtering, washing and drying solids generated by standing to obtain the crystals. According to the method, the zinc borate whisker mother liquor is mother liquor obtained in a 4ZnO.B2O3.H2O zinc borate preparation process, and contains great amounts of zinc ions and polybrate anions, great waste may be caused if the zinc ions and the polybrate anions cannot be utilized, and when the mother liquor is used for preparing the Zn3B10O18.14H2O crystals as a raw material, the mother liquor can be fully utilized, material waste can be reduced, and the preparation cost of the zinc borate crystals can be lowered.

Description

A kind of zinc borate crystal whisker mother liquor is for the preparation of the method for zinc borate crystal
Technical field
The present invention relates to field of inorganic materials, be specifically related to a kind of zinc borate crystal whisker mother liquor for the preparation of the method for zinc borate crystal.
Background technology
Along with scientific and technical development, chemical building material plastic working product and synthetic materials are applied to the fields such as building, traffic, electrical equipment, communication more and more widely.Because such materials of the overwhelming majority are inflammable or flammable, and when burning produce a large amount of poisonous, corrosive gas and flue dust, this is just to the hidden danger of having buried of all kinds of fire.So research and development fire retardant material, reduces or avoids the generation of fire failure effectively, is subject to gradually the attention of countries in the world.
Fire retardant of a great variety, its chemical structure and using method are also different.Fire retardant can be divided into organic fire-retardant and inorganic combustion inhibitor.Wherein, inorganic combustion inhibitor is nontoxic, corrosion-free, and non-secondary pollution during burning also has the premium propertiess such as good thermostability, non-volatility, becomes gradually the main flow of research and development application.Along with the continuous proposition of new environmental requirement and rules, boron flame retardant is with its good flame retardant properties, low toxicity and press down the concern that cigarette characteristic is just more and more subject to people in recent years.
Zinc borate is as a kind of novel inorganic additive flame retardant, have fire-retardant, press down cigarette, environmental protection and heat decomposition temperature advantages of higher, be one of efficient flame-retarding agent having huge market potential.Zinc borate and derivative thereof can be expressed as xZnOyB with chemical formula 2o 3zH 2o, some common zinc borate molecular formula are as follows: ZnOB 2o 32H 2o, 2ZnO3B 2o 33H 2o, 2ZnO3B 2o 37H 2o, 2ZnO3B 2o 33.5H 2o, 4ZnOB 2o 3h 2o etc.
At present, although open a large amount of synthetic methods about zinc borate in prior art, for example CN101514002A discloses a kind of method of preparing super-fine anhydrous zinc borate, utilizing nano level zinc borate and organic material is raw material, by heating, revolve steaming, stirring, the operation such as centrifugal and dry, finally obtain super-fine anhydrous zinc borate powder.CN101298333A discloses a kind of 2ZnO2B 2o 33H 2the preparation method of O zinc borate, utilizes Zinc Sulphate Heptahydrate, boric acid to react with ammoniacal liquor or sodium hydroxide, obtains the said products.CN102226299A discloses a kind of New hydrothermal synthesis method of zinc borate whisker, utilizes borax and zinc salt reaction, finally makes zinc borate crystal whisker powder.Conventionally, in the process of synthetic zinc borate, in the residue mother liquor after product filters, often contain a lot of unreacteds raw material completely, if be not used, can cause raw material to waste greatly.
In prior art, relevant Zn 3b 10o 1814H 2the synthetic method of O and application report mainly concentrate on the reaction of borax, boric acid and zinc sulfate, but take, synthesize the residue mother liquor that produces in the process of zinc borate and prepare Zn as raw material 3b 10o 1814H 2o, yet there are no bibliographical information.
Summary of the invention
In order to solve the problems of the technologies described above, the recycling method of a kind of zinc borate product residue mother liquor is after filtering provided, the inventor, after carrying out a large amount of creative works, has completed the present invention.
The invention provides a kind of zinc borate crystal whisker mother liquor for the preparation of the method for zinc borate crystal, described zinc borate crystal whisker mother liquor is for the preparation of Zn 3b 10o 1814H 2o crystal, prepares described Zn 3b 10o 1814H 2the method of O crystal comprises the following steps:
In described zinc borate crystal whisker mother liquor, add water to form mixing solutions, wherein the weight of water is 1%～40% of zinc borate crystal whisker mother liquor weight;
1h～24h is reacted in the water-bath that described mixing solutions is placed in to 20 ℃～90 ℃;
By standing 7 days～14 days of reacted described mixing solutions;
By the solid filtering of standing generation, washing, dry, obtain described Zn 3b 10o 1814H 2o crystal.
Further, by after the solid filtering of described generation, obtain remaining filtrate, using described remaining filtrate as preparation Zn 3b 10o 1814H 2the raw material of O crystal, mixes with described zinc borate crystal whisker mother liquor, for the preparation of described Zn 3b 10o 1814H 2o crystal.
Further, described zinc borate crystal whisker mother liquor is at preparation 4ZnOB 2o 3h 2in the process of O zinc borate, after the product making is filtered, the mother liquor obtaining.
Further, prepare described 4ZnOB 2o 3h 2the method of O zinc borate is: it is 2.0%～5.8% solution that borax is mixed with to mass percentage concentration; In this solution, adding mass percentage concentration is 13%～40% zinc solution, after stirring, obtains slip; Described slip is placed in reactor, regulates compactedness to 40%～90% in described reactor, described reactor is warming up to 110 ℃～160 ℃, after isothermal reaction 1h～50h, be cooled to room temperature, obtain white depositions; White depositions is filtered, washed, dry, obtain zinc borate crystal whisker powder, remaining mother liquor is described zinc borate crystal whisker mother liquor; The mol ratio of described zinc salt and described borax is 1.6:1～2.6:1.
Further, described Zn 3b 10o 1814H 2the crystal morphology of O is fibrous.
Alternatively, by the solid filtering of standing generation, washing, 40 ℃～60 ℃ oven dry, obtain described Zn 3b 10o 1814H 2o crystal.
Beneficial effect of the present invention is:
1, make full use of material, save cost, environmental protection.In the method for the invention, zinc borate crystal whisker mother liquor is preparation 4ZnOB 2o 3h 2in O zinc borate process, through product, filter the mother liquor obtaining.In this mother liquor, contain a large amount of zine ions and the complex anion of boron oxygen, using it as raw material, prepare zinc borate crystal, can utilize fully this mother liquor, reduce the waste of material, save the cost of preparing zinc borate crystal.
In addition, after making zinc borate crystal, remaining filtrate is again rendered in zinc borate crystal whisker mother liquor and is reused, and makes whole preparation process not have unnecessary waste material to produce, and environmental protection is pollution-free.
2, the pattern of product and functional.The Zn making by present method 3b 10o 1814H 2o crystal, pattern rule, size distribution is even, and its crystal morphology is fibrous, and the zinc borate of this pattern is better than granular zinc borate for the physical strength of matrix material.
3, method is simple, workable.Only by simply adding the operations such as water, heating, can obtain the Zn that pattern is good 3b 10o 1814H 2o crystal, method is simple, workable.
Accompanying drawing explanation
Fig. 1 is that the inventive method is prepared Zn 3b 10o 1814H 2the process flow sheet of O crystal.
Fig. 2 is Zn prepared by the inventive method 3b 10o 1814H 2the XRD diffractogram of O crystal.
Fig. 3 is Zn prepared by the inventive method 3b 10o 1814H 2the SEM electronic scanning figure of O crystal.
Embodiment
Below in conjunction with accompanying drawing, the present invention is described in detail by specific embodiment, should be understood that, these embodiments are only used for exemplifying the present invention, not real protection scope of the present invention are formed to any type of any restriction.
Preparation example
It is that 4.25% solution is in there-necked flask that borax is mixed with to mass percentage concentration; In this solution, adding mass percentage concentration is 33% solution of zinc sulfate, and the mol ratio of adjusting zinc sulfate and borax is 1.6:1, after stirring, obtains slip; Slip is placed in 0.5L reactor, regulates compactedness to 70% in reactor, and described reactor is warming up to 120 ℃, after isothermal reaction 16h, be cooled to room temperature, obtain white depositions, after ageing 8h, open still sampling; White depositions is filtered, washed, dry, obtain zinc borate crystal whisker powder, after filtering, remaining mother liquor is zinc borate crystal whisker mother liquor.
As shown in Figure 1, adopt above zinc borate crystal whisker mother liquor to prepare Zn 3b 10o 1814H 2the method of O crystal comprises the steps:
S101, to adding in described zinc borate crystal whisker mother liquor water to form mixing solutions, wherein the weight of water is 1%～40% of zinc borate crystal whisker mother liquor weight;
S102, described mixing solutions is placed in to the water-bath of 20 ℃～90 ℃ reacts 1h～24h;
S103, by standing 7 days～14 days of reacted described mixing solutions;
S104, by the solid filtering of standing generation, washing, dry, obtain described Zn 3b 10o 1814H 2o crystal.
The Zn of Fig. 2 for preparing according to above method 3b 10o 1814H 2the XRD diffractogram of O crystal.Fig. 3 is the Zn preparing according to above method 3b 10o 1814H 2the SEM electronic scanning figure of O crystal.
Embodiment 1
Preparation Zn 3b 10o 1814H 2o crystal, step is as follows:
In zinc borate crystal whisker mother liquor, add water to form mixing solutions, wherein the weight of water is 10% of zinc borate crystal whisker mother liquor weight;
1h is reacted in the water-bath that described mixing solutions is placed in to 20 ℃;
By standing 7 days of reacted described mixing solutions;
By the solid filtering of standing generation, washing, 50 ℃ of oven dry, obtain described Zn 3b 10o 1814H 2o crystal.
Embodiment 2
Preparation 2Zn 3b 10o 1814H 2o crystal, step is as follows:
In zinc borate crystal whisker mother liquor, add water to form mixing solutions, wherein the weight of water is 1% of zinc borate crystal whisker mother liquor weight;
10h is reacted in the water-bath that described mixing solutions is placed in to 90 ℃;
By standing 10 days of reacted described mixing solutions;
By the solid filtering of standing generation, washing, 40 ℃ of oven dry, obtain described 2Zn 3b 10o 1814H 2o crystal.
Embodiment 3
Preparation Zn 3b 10o 1814H 2o crystal, step is as follows:
In zinc borate crystal whisker mother liquor, add water to form mixing solutions, wherein the weight of water is 40% of zinc borate crystal whisker mother liquor weight;
24h is reacted in the water-bath that described mixing solutions is placed in to 70 ℃;
By standing 14 days of reacted described mixing solutions;
By the solid filtering of standing generation, washing, 60 ℃ of oven dry, obtain described Zn 3b 10o 1814H 2o crystal.
The above is only the application's embodiment; it should be pointed out that for those skilled in the art, do not departing under the prerequisite of the application's principle; can also make some improvements and modifications, these improvements and modifications also should be considered as the application's protection domain.

Claims (5)

1. zinc borate crystal whisker mother liquor, for the preparation of a method for zinc borate crystal, is characterized in that, described zinc borate crystal whisker mother liquor is for the preparation of Zn 3b 10o 1814H 2o crystal, prepares described Zn 3b 10o 1814H 2the method of O crystal comprises the following steps:
In described zinc borate crystal whisker mother liquor, add water to form mixing solutions, wherein the weight of water is 1%～40% of zinc borate crystal whisker mother liquor weight;
1h～24h is reacted in the water-bath that described mixing solutions is placed in to 20 ℃～90 ℃;
By standing 7 days～14 days of reacted described mixing solutions;
By the solid filtering of standing generation, washing, dry, obtain described Zn 3b 10o 1814H 2o crystal.
2. method according to claim 1, is characterized in that, by after the solid filtering of described generation, obtains remaining filtrate, using described remaining filtrate as preparation Zn 3b 10o 1814H 2the raw material of O crystal, mixes with described zinc borate crystal whisker mother liquor, for the preparation of described Zn 3b 10o 1814H 2o crystal.
3. method according to claim 1 and 2, is characterized in that, described zinc borate crystal whisker mother liquor is at preparation 4ZnOB 2o 3h 2in the process of O zinc borate, after the product making is filtered, the mother liquor obtaining.
4. method according to claim 1 and 2, is characterized in that, described Zn 3b 10o 1814H 2the crystal morphology of O is fibrous.
5. method according to claim 1 and 2, is characterized in that, by the solid filtering of standing generation, washing, 40 ℃～60 ℃ oven dry, obtain described Zn 3b 10o 1814H 2o crystal.
CN201410384292.3A 2014-08-06 2014-08-06 A kind of zinc borate crystal whisker mother liquor is for the preparation of the method for zinc borate crystal Active CN104150502B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201410384292.3A CN104150502B (en) 2014-08-06 2014-08-06 A kind of zinc borate crystal whisker mother liquor is for the preparation of the method for zinc borate crystal

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201410384292.3A CN104150502B (en) 2014-08-06 2014-08-06 A kind of zinc borate crystal whisker mother liquor is for the preparation of the method for zinc borate crystal

Publications (2)

Publication Number Publication Date
CN104150502A true CN104150502A (en) 2014-11-19
CN104150502B CN104150502B (en) 2016-02-24

Family

ID=51876173

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201410384292.3A Active CN104150502B (en) 2014-08-06 2014-08-06 A kind of zinc borate crystal whisker mother liquor is for the preparation of the method for zinc borate crystal

Country Status (1)

Country Link
CN (1) CN104150502B (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107829137A (en) * 2017-10-27 2018-03-23 中国科学院理化技术研究所 New application of zinc borate single crystal as semiconductor film substrate

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3002810A (en) * 1960-05-13 1961-10-03 United States Borax Chem Method for producing sodium borates of lowered iron content
US4022871A (en) * 1974-12-16 1977-05-10 Solvay & Cie Process for the fabrication of sodium bicarbonate and boric acid from borosodium ores
CN101318135A (en) * 2008-07-03 2008-12-10 浙江大学 Preparation method of visible light-responsive zinc ferrite nanocrystalline sol
CN101704532A (en) * 2009-11-10 2010-05-12 武汉大学 Preparation method of zinc borate
CN101880912A (en) * 2010-03-18 2010-11-10 中国人民解放军第二炮兵工程学院 A kind of aluminum hydroxide/magnesium-based hydrotalcite composite-phase base material and its whisker preparation method

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3002810A (en) * 1960-05-13 1961-10-03 United States Borax Chem Method for producing sodium borates of lowered iron content
US4022871A (en) * 1974-12-16 1977-05-10 Solvay & Cie Process for the fabrication of sodium bicarbonate and boric acid from borosodium ores
CN101318135A (en) * 2008-07-03 2008-12-10 浙江大学 Preparation method of visible light-responsive zinc ferrite nanocrystalline sol
CN101704532A (en) * 2009-11-10 2010-05-12 武汉大学 Preparation method of zinc borate
CN101880912A (en) * 2010-03-18 2010-11-10 中国人民解放军第二炮兵工程学院 A kind of aluminum hydroxide/magnesium-based hydrotalcite composite-phase base material and its whisker preparation method

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107829137A (en) * 2017-10-27 2018-03-23 中国科学院理化技术研究所 New application of zinc borate single crystal as semiconductor film substrate

Also Published As

Publication number Publication date
CN104150502B (en) 2016-02-24

Similar Documents

Publication Publication Date Title
CN109517220B (en) Preparation method of nano tin-based intumescent flame retardant
CN112812372B (en) Tannin-phosphazene network functionalized hydrotalcite-based flame retardant and preparation method thereof
CN103059341B (en) A functionalized hydrotalcite-like substance with fluorescence and flame retardancy and its preparation method
CN110105298A (en) A kind of synthesis of nitrogenous sulphur synergistic flame-retardant compound and its preparation method of intercalation modifying hydrotalcite
CN108485351A (en) A kind of aqueous suppression cigarette expanding fire-proof paint and preparation method thereof based on modified hydrotalcite
CN102275958A (en) Method for preparing magnesium hydroxide utilizing magnesium sulfate as raw material
CN104150502B (en) A kind of zinc borate crystal whisker mother liquor is for the preparation of the method for zinc borate crystal
CN113636565B (en) Method for preparing industrial vermiculite by phlogopite at normal pressure and industrial vermiculite
CN103172666A (en) Preparation method of dialkyl phosphinate with high thermal stability
CN102515259A (en) A method for synthesizing zinc hexahydroxystannate by utilizing nitric acid type tin stripping wastewater
CN104150501A (en) Method for preparing zinc borate crystals by using zinc borate whisker mother liquor
CN103950981B (en) A kind of preparation method of zinc molybdate micro mist
CN103086488B (en) Method for preparing flocculating agent, namely polyaluminum ferric silicate from galvanized sludge and iron tailings
CN102212868A (en) New method for preparing zinc borate whisker by hydrothermal process
CN102550557A (en) Synthesis of novel agricultural bactericide
CN107902660B (en) Method for preparing SiO2-based ATO conductive powder material from yellow phosphorus slag
CN105668596B (en) The method that template-mediated/precipitation from homogeneous solution prepares en plaque basic magnesium carbonate
CN102877115A (en) Preparation method of whisker-shaped magnesium hydroxide
CN113184885B (en) Preparation method of graphite-phase carbon nitride/phenylphosphonic acid intercalated hydrotalcite flame retardant based on phosphorus tailings
CN103318937A (en) Production method of continuously industrialized metal doped zinc hydroxystannate microencapsulated calcium carbonate
CN104402824B (en) For cobalt compound, preparation method and the sewage-treating agent thereof of sewage disposal
CN102417189B (en) Synthesis method of columnar zinc borate
CN106495233B (en) Hedgehog shape needle-like ferroso-ferric oxide and preparation method thereof
CN106745341A (en) The hydrothermal synthesis method of Carbon Dioxide nickel
CN115595666B (en) Monodisperse 517 type basic magnesium sulfate whisker and preparation method thereof

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant