CN101343774A - Preparation of hydrophobic nature nano boric acid copper crystal whisker with in situ one-step method - Google Patents
Preparation of hydrophobic nature nano boric acid copper crystal whisker with in situ one-step method Download PDFInfo
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- CN101343774A CN101343774A CNA2008100511158A CN200810051115A CN101343774A CN 101343774 A CN101343774 A CN 101343774A CN A2008100511158 A CNA2008100511158 A CN A2008100511158A CN 200810051115 A CN200810051115 A CN 200810051115A CN 101343774 A CN101343774 A CN 101343774A
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Abstract
The invention adopts the technical proposal that: 0.1 to 1.0 mol/l of borax solution of a certain volume is filled in a reactor, a negative ion surface active agent accounting for 1 to 4 percent of the borax is added, after being evenly mixed, copper salt with the intensity of 1 to 2 mol/l is added according to the material feeding ratio, the mixture is mixed, the temperature is increased to 50 to 95 DEG C, the mixing is performed under the constant temperature, the crystallizing reaction lasts for 5 to 12 hours, after filtering, cleaning, dehydrating and drying treatments at the temperature of 60 to 120 DEG C, the nanometer copper borate crystal whisker powder with the diameter of 200 to 500 nm, the length of 10 to 100 micron, and the length-diameter ratio of 20 to 500 is obtained, and the contact angle is 100 to 140 degrees. The invention has the advantages that the preparation process is simple, the nanometer copper borate crystal whisker can be finally produced, a fluxing agent is not required like other crystal whisker preparation methods, high temperature scarifying is not required, therefore pollution can not be generated, and the product manufactured through the nanometer copper borate crystal whisker preparation method has higher economic value and social value.
Description
Technical field
The present invention relates to a kind of hydrophobicity copper borate Preparation of Whiskers method, be specifically related to a kind of novel method of atmospheric low-temperature liquid phase in-situ preparing hydrophobicity copper borate whisker.
Background technology
Energy dilemma brings the fact of serious threat to cause global extensive concern to human survival, and national governments and relevant departments have dropped into huge fund and manpower and materials, seek a solution for a problem.But position up till now, the human new forms of energy that can replace oil, coal resources that also do not find.The task of top priority has human necessary solution of two things, and the one, reduce consumption to existing resource, postpone the exhausted time that arrives of non-renewable energy as far as possible, the 2nd, develop renewable new forms of energy minimizing or replace human dependence nonrenewable resource.
Boron is a kind of broad-spectrum chemical industry mineral, and the compound of boron and boron is widely used in chemical industry, metallurgy, opticglass, national defence, nuclear power, medicine, rubber and light industrial segment.On chemical industry, in order to all cpds and the element boron of system borax, boric acid, boron; In the metallurgical industry, be used for smelting boron steel; In the national defence space industry, the compound of boron and hydrogen, lithium, beryllium etc. can burn, and is the high energy rocket engine fuel; In the process of making glass, add an amount of borax or boric acid, can reduce the coefficient of expansion of glass, improve thermostability, increase gloss and transparency; Borax is still produced one of enamelled main raw material; In recent years, boric acid is used for the manufacturing of glass fibre in a large number.
Boron rock is a kind of important chemical material, and its direct purposes is to make borax and boric acid, in addition, also is used for fields such as smelting boron steel, abrasive substance, sanitas, coating, boron fertilizer and agricultural chemicals.China's boron resource is abundanter, but utilizable reserves deficiency can not satisfy following needs fully.Along with the development of Chinese national economy, the demand of boron is still increasing, and the available boron rock reserves of China can not satisfy following needs fully.Therefore protecting and rationally utilize boron resource is the important step of China's boron industrial sustainable development strategy, also is the puzzlement that scarcity of resources is broken away from China's boron industry, strengthens the task of top priority of existence and competitive capacity.
In recent years, Chinese scholars has been carried out a series of research work aspect the matrix material reinforcement.They studies show that whisker except that having high-intensity performance, have the performance that keeps hot strength, and whisker also has some special magnetic, electrical and optical property than superalloy loss of strength much less commonly used during high temperature, can be developed as functional materials.Whisker mainly as the toughener of matrix material, is used for aerospace flight vehicle member and parts, also is applied in machinery, automobile, chemical industry, biomedicine and dairy industry, thereby has opened up a new field, forward position.
Crystal whisker materials can be divided into organic crystalline must and inorganic crystal whisker two big classes, wherein inorganic crystal whisker is as a kind of novel strongthener, has high strength, heat-resisting, wear-resisting, protection against corrosion, vibration damping, damping, suction ripple, many special advantages and function such as fire-retardant.Can be used in the polymkeric substance such as thermosetting resin, thermoplastic resin, rubber; Can produce high performance engineering plastics, matrix material, tackiness agent, coating etc.There is the investigator to point out, inorganic crystal whisker is filled in the polymkeric substance, might obtain polymkeric substance whisker mixture truly, this novel mixture, rigidity, dimensional stability and the thermostability of inorganic crystal whisker can be combined with the toughness of macromolecular material, be expected to produce the required material of new and high technology and open up, enlarge the range of application that has macromolecular material now, this field has become the focus of domestic and international research, has wide application and market outlook.
Some domestic Preparation of Whiskers methods mainly contain hydrothermal method and solid phase method, and these two kinds of methods all have limitation, and the former has relatively high expectations to laboratory apparatus, need to use reactor to finish experiment, and yield poorly, the operation of equipment complexity has strengthened cost virtually; The latter then needs by high-temperature calcination, and this can make the particle diameter of product increase inevitably, and the high-temperature roasting energy consumption is big, production cycle is long, and use fusing assistant that cost is increased, the whisker quality of the easy contaminate environment of Pai Fang gas, and gained simultaneously is not as hydrothermal method.Therefore, these unfavorable factors can make that all the economic benefit of product and social benefit incur loss.
In the present invention, our reasonable use boron resource, original position one step precipitator method synthesizing hydrophobic copper borate whisker.The copper borate whisker is an inorganics, can not be fine compound with polymkeric substance, copper borate whisker after the finishing had both had the character of whisker in the method for the invention, has hydrophobic lipophilicity again, modification by tensio-active agent, can improve whisker and whisker be combined with polymkeric substance with stronger bond valence power, thereby reach the enhanced effect with the consistency of polymkeric substance.And the synthesis technique of the original position one step precipitator method is simple, and starting material are few, is indubitable to the saving of the resource and the energy, and can not brings environmental protection pressure.
Summary of the invention
Purpose of the present invention just provides that a kind of production technique is simple, cost is low, reaction process is pollution-free, at atmospheric low-temperature liquid phase made acid-stable in situ nano boric acid copper whisker.
Technical scheme of the present invention is: certain volume 0.1～1.0mol/l borax soln is placed reactor, add the anion surfactant that accounts for borax 1～4%, after stirring, add the mantoquita that concentration is 1～2mol/l again by feed ratio, stirring is warming up to 50～95 ℃, constant temperature stirring reaction crystallization 5～12h, after filtration, washing, dehydration, 60～120 ℃ of following drying treatment, obtaining diameter is 200～500nm, length is 10～100 μ m, length-to-diameter ratio is 20～500 nano boric acid copper whisker powder, its contact angle is 100～140 degree, the characteristics of the inventive method are that preparation technology is simple, finally can make nano boric acid copper whisker, and need use fusing assistant when preparing unlike other whiskers, do not need high-temperature calcination equipment to calcine yet, thereby can not produce pollution, and do not use reactor, simplify technology, reduce cost, these all make the product for preparing with the inventive method have higher economic value and social value.
Further set forth the present invention below in conjunction with specific embodiment.
Embodiment 1:
1. adding the 50ml molar content in there-necked flask is the Na of 0.1mol/l
2B
4O
710H
2O puts into 50 ℃ of water-baths, and the adding tensio-active agent also stirs;
2. the copper salt solution that under agitation, adds 20ml 1mol/l;
3. maintenance temperature continues to stir 5h;
4. filter washing upper strata product;
5.60 ℃ dehydrate, obtaining diameter after the grinding is 500nm, length is 10 μ m, and length-to-diameter ratio is 20 copper borate powder;
Embodiment 2:
1. adding the 50ml molar content in there-necked flask is the Na of 0.1mol/l
2B
4O
710H
2O puts into 70 ℃ of water-baths, and the adding tensio-active agent also stirs;
2. the copper salt solution that under agitation, adds 20ml 1mol/l;
3. maintenance temperature continues to stir 5h;
4. filter washing upper strata product;
5.60 ℃ dehydrate, obtaining diameter after the grinding is 500nm, length is 30 μ m, and length-to-diameter ratio is 60 copper borate powder;
Embodiment 3:
1. adding the 50ml molar content in there-necked flask is the Na of 0.1mol/l
2B
4O
710H
2O puts into 90 ℃ of water-baths, and the adding tensio-active agent also stirs;
2. the copper salt solution that under agitation, adds 20ml 1mol/l;
3. maintenance temperature continues to stir 7h;
4. filter washing upper strata product;
5.60 ℃ dehydrate, obtain the copper borate whisker powder of pattern homogeneous after the grinding, by the contact angle test, the products therefrom contact angle is 100 degree, and by scanning electron microscope as can be known, the diameter of product is 500nm, and length is 60 μ m, and length-to-diameter ratio is 120;
Embodiment 4:
1. adding the 50ml molar content in there-necked flask is the Na of 0.1mol/l
2B
4O
710H
2O puts into 90 ℃ of water-baths, and the adding tensio-active agent also stirs;
2. the copper salt solution that under agitation, adds 20ml 1mol/l;
3. maintenance temperature continues to stir 9h;
4. filter washing upper strata product;
5.60 ℃ dehydrate, obtain the copper borate crystal whisker powder of pattern homogeneous after the grinding, and to record its diameter be 200nm, length is 60 μ m, and length-to-diameter ratio is 300, and by the contact angle test, the products therefrom contact angle is 100 degree;
Embodiment 5:
1. adding the 50ml molar content in there-necked flask is the Na of 0.1mol/l
2B
4O
710H
2O puts into 90 ℃ of water-baths, and the adding tensio-active agent also stirs;
2. the copper salt solution that under agitation, adds 20ml 1mol/l;
3. maintenance temperature continues to stir 9h;
4. filter washing upper strata product;
5.80 ℃ dehydrate, obtain the copper borate crystal whisker powder of pattern homogeneous after the grinding, and to record the product diameter be 200nm, length is 80 μ m, and length-to-diameter ratio is 400, and by the contact angle test, the products therefrom contact angle is 120 degree;
Embodiment 6:
1. adding the 50ml molar content in there-necked flask is the Na of 0.1mol/l
2B
4O
710H
2O puts into 90 ℃ of water-baths, and the adding tensio-active agent also stirs;
2. the copper salt solution that under agitation, adds 20ml 1mol/l;
3. maintenance temperature continues to stir 9h;
4. filter washing upper strata product;
5.100 ℃ dehydrate, obtain the copper borate crystal whisker powder of pattern homogeneous after the grinding, and record product 200nm, length is 100 μ m, and length-to-diameter ratio is 500, and by the contact angle test, the products therefrom contact angle is 140 degree;
Claims (4)
1. novel method for preparing hydrophobic type copper borate whisker, the steps include: certain volume 0.1～1.0mol/l borax soln is placed reactor, add the anion surfactant that accounts for borax 1～4%, after stirring, add the mantoquita that concentration is 1～2mol/l again by feed ratio, stirring is warming up to 50～95 ℃, constant temperature stirring reaction crystallization 5～12h, after filtration, washing, dehydration, 60～120 ℃ of following drying treatment, obtaining diameter is 200～500nm, length is 10～100 μ m, length-to-diameter ratio is 20～500 nano boric acid copper whisker powder, and its contact angle is 100～140 degree.
2. a kind of novel method for preparing hydrophobic type copper borate whisker described in right 1 is characterized in that: described anion surfactant can be a kind of in oleic acid, stearic acid, phosphoric acid ester, Witco 1298 Soft Acid and the corresponding salt.
3. a kind of novel method for preparing hydrophobic type copper borate whisker described in right 1 is characterized in that: mantoquita can be a kind of in copper sulfate, cupric chloride, the cupric nitrate.
4. a kind of novel method for preparing hydrophobic type copper borate whisker described in right 1, it is characterized in that: the mol ratio of boron and cupric ion is 1: 2～4.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008100511158A CN101343774A (en) | 2008-08-26 | 2008-08-26 | Preparation of hydrophobic nature nano boric acid copper crystal whisker with in situ one-step method |
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| Application Number | Priority Date | Filing Date | Title |
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| CNA2008100511158A CN101343774A (en) | 2008-08-26 | 2008-08-26 | Preparation of hydrophobic nature nano boric acid copper crystal whisker with in situ one-step method |
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| CN101343774A true CN101343774A (en) | 2009-01-14 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102126730A (en) * | 2010-12-13 | 2011-07-20 | 聊城大学 | Method for preparing copper borate/SiO2 composite particles |
| CN107686662A (en) * | 2017-10-25 | 2018-02-13 | 浙江威思康塑胶有限公司 | A kind of environment friendly flame retardant |
| CN107686661A (en) * | 2017-10-25 | 2018-02-13 | 浙江威思康塑胶有限公司 | A kind of preparation method of cable fire retardant |
| CN108003621A (en) * | 2017-11-30 | 2018-05-08 | 长兴科创科技咨询有限公司 | A kind of Preen nono fire proofing |
| CN112374508A (en) * | 2020-11-02 | 2021-02-19 | 中山大学 | Amorphous nickel borate nanosheet and preparation method and application thereof |
-
2008
- 2008-08-26 CN CNA2008100511158A patent/CN101343774A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102126730A (en) * | 2010-12-13 | 2011-07-20 | 聊城大学 | Method for preparing copper borate/SiO2 composite particles |
| CN102126730B (en) * | 2010-12-13 | 2012-12-12 | 聊城大学 | Method for preparing copper borate/SiO2 composite particles |
| CN107686662A (en) * | 2017-10-25 | 2018-02-13 | 浙江威思康塑胶有限公司 | A kind of environment friendly flame retardant |
| CN107686661A (en) * | 2017-10-25 | 2018-02-13 | 浙江威思康塑胶有限公司 | A kind of preparation method of cable fire retardant |
| CN108003621A (en) * | 2017-11-30 | 2018-05-08 | 长兴科创科技咨询有限公司 | A kind of Preen nono fire proofing |
| CN112374508A (en) * | 2020-11-02 | 2021-02-19 | 中山大学 | Amorphous nickel borate nanosheet and preparation method and application thereof |
| CN112374508B (en) * | 2020-11-02 | 2022-07-12 | 中山大学 | Amorphous nickel borate nanosheet and preparation method and application thereof |
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Open date: 20090114 |