CN101418139A - Magnesium hydroxide/TiO2 composite material with flame resistance property and pigment - Google Patents
Magnesium hydroxide/TiO2 composite material with flame resistance property and pigment Download PDFInfo
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- CN101418139A CN101418139A CNA2007101656041A CN200710165604A CN101418139A CN 101418139 A CN101418139 A CN 101418139A CN A2007101656041 A CNA2007101656041 A CN A2007101656041A CN 200710165604 A CN200710165604 A CN 200710165604A CN 101418139 A CN101418139 A CN 101418139A
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Abstract
The invention provides a magnesium hydroxide/TiO2 composite material with fire resistance and pigment properties and a preparation method thereof. The preparation method adopts magnesium hydroxide powder as a core substrate and crystal TiO2 as a coating, realizes reaction coating and modification of the TiO2 on the surface of the core substrate in a wet superfine grinding system by means of grain-grain coating modification, so as to prepare the magnesium hydroxide/TiO2 composite material with the fire resistance and the pigment properties. The TiO2 in the composite material is uniformly coated on the surface of magnesium hydroxide particles and stably combined with the magnesium hydroxide particles. The magnesium hydroxide/TiO2 composite material has the pigment properties such as strong covering power and good compatibility with an application system. Simultaneously, the magnesium hydroxide/TiO2 composite material prepared has the fire resistance due to the fire resistance of magnesium hydroxide. Moreover, the magnesium hydroxide/TiO2 composite material also has the characteristics of simple manufacturing technique, low cost and so on, can obtain the same technical pigment properties with use of titanium pigment powder when being applied to products such as coating, greatly reduces the cost, can also be used in occasions which utilize the physical property and the fire resistance of white pigment such as plastics and rubber, and has the functions of improving the applied product performance and reducing the cost.
Description
Affiliated technical field
The present invention relates to and utilize the preparation of mineral-modified and compounding technology to have the production technical field of the matrix material of flame-retardant nature and pigment property, specifically, relate to magnesium hydroxide/TiO
2The preparation method of matrix material.
Background technology
Titanium dioxide (pigmentary titanium dioxide) has obtained to widely apply at numerous industrial sectors such as coating, papermaking, plastics, thereby has become important chemical material in the development of the national economy as the color superfine white pigment of people's manufacturing up to now.In the last few years, because of the construction industry of factors such as Economic development, social progress and people's living standard raising drive and the fast development of relevant paint industry, the demand of white pigment titanium dioxide was grown with each passing day.And on the other hand, the shortage day by day of world's high-quality titanium resource, the resources processing process complications, the environmental protection requirement strictness, these all cause the titanium white production cost to increase, and price raises up.The problems referred to above constantly increase the weight of titanium white consumption industry such as coating burden, and therefore industry development is restricted.
Magnesium hydrate powder is the halogen-free flame retardants that industries such as plastics, rubber are used, and has Halogen, nontoxic, eco-friendly characteristics such as burning the time is not fuming, non-corrosiveness gas release.
It is to solve in-problem effective way in titanium white production and the consumption that the modification of employing inorganic materials prepares the composite product similar and with low cost to the titanium white performance to compounding technology.By inorganic surfaces coating modification mode, coat TiO at inorganic material surfaces such as non-metallic mineralss
2Layer and form composite white pigment and receive concern both domestic and external always with TiO 2 pigment character, and formed main with inorganic precipitation reaction-thermal treatment crystallization method and dry conditions grain-two kinds of technological methods that prepare composite pigment of grain coating modification method.
Specifically being characterized as of inorganic precipitation reaction-thermal treatment crystallization method: will place as the nonmetalliferous ore composition granule of matrix in the hydrolyzation system of titanium salt (mainly being titanyl sulfate), and cause the titanium salt hydrolysis, and generate hydrated titanium dioxide (TiO
2H
2O) cover the mineral grain surface, make the TiO of composite surface again through thermal treatment
2H
2O generates crystal type TiO
2The coating thing.The problem that this method exists mainly contains: the inducing action of mineral substance bag nuclear matrix causes the hydrated titanium dioxide throw out to be difficult to generate rutile titanium dioxide by follow-up crystallization; Be subjected to the restriction of hydrolytic process titanium salt concentration and solid content, coat TiO
2Amount and degree of uniformity are restricted, and the pigment performance of product does not generally reach requirement; The removal of impurity such as titanium salt hydrolysis and iron ion produces a large amount of acid waste waters, contaminate environment.
Dry conditions grain-grain coating modification method is with TiO
2Place mechanical stirring system with non-metallic minerals, realize fine particle TiO by effects such as mechanical dispersion, impact shear with dry type shock action
2Coating at thicker non-metallic minerals particle surface.Adopt this method, because of bag nuclear matrix and TiO
2Degree of scatter relatively poor, what lack the firmly effect that produces between matrix and the titanium white excites external force and binding groups thereby mixture pigment performance difference and instability.
Summary of the invention
The purpose of this invention is to provide a kind of at magnesium hydroxide particle surface firm coating crystallization TiO
2Particle is a feature and because of upper layer TiO
2Character and TiO
2Have pigmentary titanium dioxide character and composite white pigment with low cost with the comprehensive action of magnesium hydroxide performance; Simultaneously, since the flame retardant properties of magnesium hydroxide itself, magnesium hydroxide/TiO
2Matrix material has corresponding flame retardant properties.
The present invention has realized magnesium hydroxide/TiO by following measure
2Crystallization TiO in the matrix material
2Particle coats firmly and uniformly on the magnesium hydroxide particle surface:
(1) adopt the wet ultra-fine grinding method will be as the magnesium hydroxide particle of bag nuclear thing with as the crystallization TiO of coating thing
2Particle is refined to the size range that both are complementary respectively, i.e. bag nuclear composition granule diameter (ball-type equivalent diameter): TiO
2Particle diameter is about 5-10: 1;
(2) make magnesium hydroxide particle produce mechanical force surface active effect by extra-fine grinding, promote itself and TiO with this
2Between reaction bonded;
(3) magnesium hydroxide particle and TiO
2Each self-forming surface functional group in reaction system is realized the alternate reaction of two particulate by the chemical bonding between functional group;
Magnesium hydroxide/the TiO of the present invention's preparation
2Matrix material is because of particle surface TiO
2Strong dissemination that the high refractive index of coating layer, heterogeneous particulate material cause and high scattering process, and wrap up the strong covering effect that more air dielectric causes when forming coating and have the pigment property of similar titanium dioxide.Simultaneously, because the character of magnesium hydroxide itself, and make magnesium hydroxide/TiO
2Matrix material has the character of fire retardant when using in polymkeric substance such as plastics, rubber.
Magnesium hydroxide/the TiO of the present invention's preparation
2Matrix material is owing to wherein only contain part TiO
2, and solid bag nuclear thing magnesium hydroxide relative low price, so its cost is compared with titanium dioxide and is greatly diminished.
Final magnesium hydroxide/the TiO that forms of the present invention
2The composition of matrix material with consist of: magnesium hydroxide 45%-85%, crystallization TiO
2(anatase titanium dioxide or rutile-type) 15%-55%.
Realize magnesium hydroxide/TiO of the present invention
2The concrete preparation method of matrix material is:
Raw material selection:
1. magnesium hydrate powder is selected the natural brucite powder for use, fineness 200-1250 order, and mineral purity is greater than 80%;
2. anatase titanium dioxide or Rutile type Titanium Dioxide industrial goods (crystallization TiO
2), whiteness is greater than 95%;
3. sodium polyacrylate (the above rank of technical pure) is mixed with the aqueous solution with deionized water, and strength of solution 20% is at magnesium hydroxide and TiO
2Add use as dispersion agent during powder slurrying.
The concrete steps of principle production process are:
One, at first forms the requirement of solid content 30%～60% in the suspensoid by magnesium hydrate powder and water, take by weighing magnesium hydrate powder, water and account for the sodium polyacrylate of dry powder amount 0.5%-1.2%, place wet type to stir in the extra-fine grinding system of mill, stir to make by stirrer and treat the extra-fine grinding slurry with high-speed stirring effect;
Two, by crystallization TiO
2(anatase titanium dioxide or rutile-type) and water form the requirement of solid content 50%～70% in the suspensoid, take by weighing TiO
2, water and account for the sodium polyacrylate of dry powder amount 0.3%-2%, place in the stirrer with high-speed stirring effect and stir, make slurry;
Three, start the extra-fine grinding system that wet type stirs mill, the slurry that magnesium hydroxide and water are made carries out grinding operation, makes levigate product granularity be less than 1 μ m content 60%～75%, and with itself and TiO
2Slurry mixes stirring, and both blending ratios (dry powder weight) are pressed TiO
2/ (magnesium hydroxide+TiO
2The requirement of)=15%-55% is determined.Then mixture slurry is stirred homogenizing;
Four, start the extra-fine grinding system that wet type stirs mill, to the TiO of homogenizing
2Slurry and magnesium hydroxide mixture slurry carry out grinding operation, make levigate product granularity be less than 2 μ m content 82%～88%, and importing has in the stirred pot of medium stirring intensity;
Five, to magnesium hydroxide/TiO is housed
2Mix in the stirred pot of ultra-fine slurry and add water, make it be diluted to solid content 15%-35%, and stir.Use the ultra-fine hydroclassifier of GSDF-25 (Φ 25) type that it is carried out classification then, make the classification overflow granularity reach-2 μ m content 87%～92%.
Six, utilize sheet frame pressure filter or whizzer that the classification overflow is filtered and form filter cake;
Seven, filter cake is placed the drying machine of 90 ℃-120 ℃ of temperature be dried to moisture below 1%;
Eight, dried material is sent in the beater handled, make it to form even-grained powder;
Embodiment
Embodiment 1:
1. magnesium hydrate powder (200 order) 400kg, deionized water 400kg are placed wet type to stir in the extra-fine grinding system of mill, stir 30min by stirrer with high-speed stirring effect, add the solution (strength of solution 20% that contains the 4kg sodium polyacrylate then, add this solution 20kg), restir 40min makes and treats the extra-fine grinding slurry;
2. start the extra-fine grinding system that wet type stirs mill, the slurry of magnesium hydrate powder and water being made according to continuous grinding mode grinds and makes levigate product granularity reach-2 μ m content 70%;
3. with crystallization TiO
2(Rutile type Titanium Dioxide) 200kg, deionized water 200kg place and stir 15min in the stirred pot with high-speed stirring effect, add the solution (strength of solution 20% adds this solution 15kg) that contains the 3kg sodium polyacrylate then, and restir 40min makes slurry;
4. with the levigate slurry 300kg of magnesium hydroxide, TiO
2Slurry 160kg mixes, and high-speed stirring 40min is to realize the homogenizing of mixture slurry;
5. start the extra-fine grinding system that wet type stirs mill, according to continuous grinding mode to the TiO of homogenizing
2Slurry and super fine magnesium hydroxide mixture slurry carry out grinding operation, make levigate product granularity be less than 2 μ m content 85%, and importing has in the stirred pot of medium stirring intensity;
6. to superfine Ti O is housed
2With add water 400kg in the stirred pot of superfine white mineral mixture slurry 400kg, and stir.Use the ultra-fine hydroclassifier of GSDF-25 (Φ 25) type that it is carried out classification then, make the classification overflow granularity reach-2 μ m content 90%;
7, utilize tripod pendulum type batch centrifugal that the classification overflow is filtered and form filter cake;
8, filter cake is placed the drying machine of 110 ℃ of temperature be dried to moisture below 1%;
9, dried material is sent in the beater handled, make it to form even-grained powder;
Embodiment 2:
1. magnesium hydrate powder (1250 order) 400kg, deionized water 400kg are placed wet type to stir in the extra-fine grinding system of mill, stir 15min by stirrer with high-speed stirring effect, add the solution (strength of solution 20% that contains the 6kg sodium polyacrylate then, add this solution 30kg), restir 40min makes and treats the extra-fine grinding slurry;
2. start the extra-fine grinding system that wet type stirs mill, the slurry of magnesium hydrate powder and water being made according to continuous grinding mode grinds and makes levigate product granularity reach-2 μ m content 70%;
3. with crystallization TiO
2(anatase thpe white powder) 200kg, deionized water 200kg place and stir 15min in the stirred pot with high-speed stirring effect, add the solution (strength of solution 20% adds this solution 15kg) that contains the 3kg sodium polyacrylate then, and restir 40min makes slurry;
4. with the levigate slurry 300kg of magnesium hydroxide, TiO
2Slurry 160kg mixes, and high-speed stirring 40min is to realize the homogenizing of mixture slurry;
5. start the extra-fine grinding system that wet type stirs mill, according to continuous grinding mode to the TiO of homogenizing
2Slurry and super fine magnesium hydroxide mixture slurry carry out grinding operation, make levigate product granularity reach-2 μ m content 85%, and importing has in the stirred pot of medium stirring intensity;
6. to superfine Ti O is housed
2With add water 400kg in the stirred pot of superfine white mineral mixture slurry 400kg, and stir.Use the ultra-fine hydroclassifier of GSDF-25 (Φ 25) type that it is carried out classification then, make the classification overflow granularity reach-2 μ m content 90%.
7, utilize tripod pendulum type batch centrifugal that the classification overflow is filtered and form filter cake;
8, filter cake is placed the drying machine of 100 ℃ of temperature be dried to water ratio＜1%;
9, dried material is sent in the beater handled, make it to form even-grained powder;
Magnesium hydroxide/the TiO that makes respectively by embodiment 1 and embodiment 2
2Performance of composites is listed in table 1, the magnesium hydroxide/TiO that uses embodiment 1 to make
2The covering performance of the exterior wall latex coating of Composite Preparation, the magnesium hydroxide/TiO that uses embodiment 2 to make
2The performance of the internal wall emulsion coating of Composite Preparation and list in table 2 with the contrast of titanium dioxide.Magnesium hydroxide/TiO with embodiment 1 and embodiment 2 preparations
2Flame retardant properties after matrix material adds among the PVC sees Table 3, and (proportioning is PVC:DOP: magnesium hydroxide/TiO
2Matrix material=100: 50: 80).
The result shows: with magnesium hydroxide/TiO
2Matrix material is as single pigment, and the opacifying power of its preparation coating is suitable with the use titanium dioxide, magnesium hydroxide/TiO
2Matrix material is with larger proportion and the compound use of titanium dioxide, and the coating opacifying power is apparently higher than using titanium dioxide.Therefore think magnesium hydroxide/TiO
2Matrix material has the pigment performance similar with titanium dioxide.As magnesium hydroxide/TiO
2During fire-retardant dose of use of matrix material, have the flame retardant properties close with magnesium hydroxide.
Magnesium hydroxide/TiO
2Performance of composites table 1
Magnesium hydroxide/TiO
2Matrix material and titanium dioxide prepare coating property (contrast ratio, %) detected result table 2
Magnesium hydroxide/TiO
2The flame retardant properties detected result table 3 of matrix material in flexible PVC
| Performance index | Not fire-retardant | Pure cerium hydroxide magnesium is fire-retardant | Magnesium hydroxide/TiO of embodiment 1 2Composite sample is fire-retardant | Magnesium hydroxide/TiO of embodiment 2 2Composite sample is fire-retardant |
| Oxygen index, % | 18 | 29 | 26 | 26 |
| Flame retardant rating | Not fire-retardant | The UL94-V0 level | The UL94-V1 level | The UL94-V1 level |
Claims (3)
1. magnesium hydroxide/TiO with flame retardant resistance and pigment
2The preparation method of matrix material is characterized in that: with the magnesium hydrate powder bag nuclear matrix, and crystallization TiO
2(anatase titanium dioxide and rutile-type) is the coating thing, adopts magnesium hydroxide wet ultra-fine grinding and magnesium hydroxide and crystallization TiO
2Approach is ground in the wet method blend, and the modes such as grain-grain coating modification reaction that refinement, surface hydroxylation transformation and Mechanochemical Effect cause of cutting apart by solid particulate are prepared from.
Requiring should be greater than 80% as magnesium hydroxide content in the magnesium hydrate powder of bag nuclear matrix, magnesium hydroxide/TiO
2The fineness of matrix material reaches-2 μ m content 87%～92%, and each component ratio of components by weight is: magnesium hydrate powder 45%-85%, crystallization TiO
2(anatase titanium dioxide or rutile-type) 15%-55%.
2. magnesium hydroxide/TiO
2Matrix material, its preparation technology and method feature are:
A, form the requirement of solid content 30%～60% in the suspensoid by magnesium hydroxide and water, take by weighing magnesium hydrate powder, water and account for the sodium polyacrylate of dry powder amount 0.5%-1.2%, place wet type to stir in the extra-fine grinding system of mill, stir to make by stirrer and treat the extra-fine grinding slurry with high-speed stirring effect;
B, by crystallization TiO
2(anatase titanium dioxide or rutile-type) and water form the requirement of solid content 50%～70% in the suspensoid, take by weighing TiO
2, water and account for the sodium polyacrylate of dry powder amount 0.3%-2.0%, place in the stirrer with high-speed stirring effect and stir, make slurry;
C, start the extra-fine grinding system that wet type stirs mill, the slurry that magnesium hydroxide and water are made carries out grinding operation, makes levigate product granularity reach-1 μ m content 60%～75%, and with itself and TiO
2Slurry mixes stirring, and both blending ratios (dry powder weight) are pressed TiO
2/ (magnesium hydroxide+TiO
2The requirement of)=15%-50% is determined, then mixture slurry is stirred homogenizing;
D, start the extra-fine grinding system that wet type stirs mill, to the TiO of homogenizing
2Slurry and magnesium hydroxide mixture slurry carry out grinding operation, make levigate product granularity reach-2 μ m content 82%～88%, and importing has in the stirred pot of medium stirring intensity;
E, to magnesium hydroxide/TiO is housed
2Mix in the stirred pot of ultra-fine slurry and add water, make it be diluted to solid content 15%-35%, and stir.Use the ultra-fine hydroclassifier of GSDF-25 (Φ 25) type that it is carried out classification then, make the classification overflow granularity reach-2 μ m content 87%～92%.
F, utilize sheet frame pressure filter or whizzer that the classification overflow is filtered to form filter cake;
G, place the drying machine of 90 ℃-120 ℃ of temperature to be dried to water ratio＜1% filter cake;
H, dried material sent in the beater handle, make it to form even-grained powder.
3. magnesium hydroxide/TiO according to claim 2
2The preparation technology of matrix material and method are characterised in that:
A, the requirement that accounts for magnesium hydrate powder 1% by magnesium hydroxide/(magnesium hydroxide+water)=50%, sodium polyacrylate, in wet type stirred the extra-fine grinding system of mill, the stirrer by the high-speed stirring effect stirs to make by what magnesium hydrate powder, water and sodium polyacrylate formed treated the extra-fine grinding slurry.Adopt in the magnesium hydrate powder magnesium hydroxide mineral content greater than 80%;
B, by crystallization TiO
2(anatase titanium dioxide or rutile-type) and water form the requirement of solid content 50% in the suspensoid, take by weighing TiO
2, water and account for the trimerization sodium phosphate of dry powder amount 1.5%, place in the stirrer with high-speed stirring effect and stir, make slurry;
C, start the extra-fine grinding system that wet type stirs mill, the slurry that magnesium hydrate powder and water are made carries out grinding operation, makes levigate product granularity reach-1 μ m content 70%, then with itself and TiO
2Slurry is pressed TiO
2/ (magnesium hydrate powder+TiO
2The requirement of)=34% mixes homogenizing;
D, utilize wet type to stir the extra-fine grinding system of mill, to the TiO of homogenizing
2Grind with the magnesium hydrate powder mixture slurry and make levigate product granularity reach-2 μ m content greater than 85%;
E, add water to superfine Ti O
2Being diluted to solid content with the super fine magnesium hydroxide mixture slurry is 25%, and dispersed with stirring evenly back is carried out classification with the ultra-fine hydroclassifier of GSDF-25 (Φ 25) type, makes the classification overflow granularity reach-2 μ m content 90%;
F, utilize whizzer or vacuum filter that the classification overflow is filtered to form filter cake;
G, to place the drying machine of 100 ℃ of temperature to be dried to filter cake moisture below 1%;
H, dried material sent in the beater handle, make it to form even-grained powder.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101656041A CN101418139A (en) | 2007-10-25 | 2007-10-25 | Magnesium hydroxide/TiO2 composite material with flame resistance property and pigment |
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|---|---|---|---|
| CNA2007101656041A CN101418139A (en) | 2007-10-25 | 2007-10-25 | Magnesium hydroxide/TiO2 composite material with flame resistance property and pigment |
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Application publication date: 20090429 |