CN1030138C - Preparation method of modified calcium aluminate - Google Patents
Preparation method of modified calcium aluminate Download PDFInfo
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- CN1030138C CN1030138C CN92112151.2A CN92112151A CN1030138C CN 1030138 C CN1030138 C CN 1030138C CN 92112151 A CN92112151 A CN 92112151A CN 1030138 C CN1030138 C CN 1030138C
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- calcium aluminate
- modified calcium
- reaction
- aluminium hydroxide
- aluminate
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/16—Preparation of alkaline-earth metal aluminates or magnesium aluminates; Aluminium oxide or hydroxide therefrom
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- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
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- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The present invention relates to a new method for preparing modified calcium aluminate, which comprises the following procedures: adding aqueous solution containing raw materials of calcium oxide and aluminium hydroxide with the molar ratio of 1.00 to 2.50 of calcium and aluminium, and surfactant with the dosage of 0.5 to 3.0 according to the weight percentage of wholly reacting materials into a reactor, and stirring and mixing the mixture of the aqueous solution and the surfactant; at reaction temperature of not lower than 60 DEG C and the reaction time of less than 10 hours, reacting and generating modified calcium aluminate. The present invention has the characteristics of short reaction time and simple technology. Because the product does not need to be washed, the pollution to the environment, which is caused by washing liquid, and the recovering problem are avoided. The adverse effects of the modified calcium aluminate on the mechanical properties of a product are greatly reduced. The flame retardant performance, the absorbing capacity to HCl and the smoke abatement performance are good.
Description
The present invention relates to the production method of calcium aluminate.
Japanese Patent Laid discloses the i.e. two sections hydrothermal synthesis methods of synthetic method that clear and 62-128919 discloses a kind of calcium aluminate: below 60 ℃, more than six hours calcium oxide, aluminium hydroxide are being carried out pre-treatment earlier, react more than 17 hours, at 90 ℃ then again with obtaining finished product behind the washing with acetone; Its shortcoming is: reaction is divided into two sections to be carried out, and total reaction time reached more than 22 or 24 hours, and reclaims and pollution problem because of using washing with acetone to cause.
The present invention has been intended to overcome the deficiency of above-mentioned prior art and has proposed a kind of production method of modified calcium aluminate.
The present invention is a kind of new modified calcium aluminate production method, be 1.00～2.50 the aqueous solution, dosage of surfactant by the weight percent of total reaction material with raw material calcium oxide and aluminium hydroxide by the mol ratio of calcium and aluminium be 0.5～3.0 to drop in the reactor and mix, be not less than 60 ℃ in temperature of reaction, reaction times is no less than 10 hours, and reaction generates modified calcium aluminate; The calcium aluminate that is generated obtains finished product after filtering, and filtrate filtered adds continuation use in the reactor again, has so not only made full use of waste liquid but also has reduced environmental pollution; Wherein the raw materials used calcium oxide of the present invention can be unslaked lime, acetylene slag, industrial lime, and raw materials used aluminium hydroxide can be industrial aluminium hydroxide; Principal feature of the present invention is to have used tensio-active agent, make reaction mass wetted rapidly at the initial reaction stage tensio-active agent, infiltration, thereby be uniformly dispersed and add fast response and carry out, help shortening the reaction times, when reaction finishes, the hydrophilic group part and the calcium aluminate combination of tensio-active agent, and hydrophobic group is partly assembled, be wrapped in the surface of calcium aluminate, thereby calcium aluminate and some macromolecular materials such as plastics that the present invention is produced, rubber etc. have a lot of consistencies, its add-on does not just have above-mentioned effect very little, and effect does not have tangible increase when too many, and tensio-active agent can be silicon-dioxide, aluminic acid lipoprotein, silane, lipid acid, titanic acid ester, zirconium aluminate.And temperature of reaction and reaction times are in order to control the abundant degree of its reaction, if temperature of reaction is lower than 60 ℃, its sufficient reacting is finished the reaction times is significantly extended, and are unfavorable for so very much suitability for industrialized production.
Reaction mass total amount among the following embodiment is 200 grams;
Embodiment 2, the aqueous solution, tensio-active agent aluminic acid lipoprotein consumption that with raw material acetylene slag and aluminium hydroxide by the mol ratio of calcium and aluminium are 2.20: 1.00 are 1.60 to drop in the reactors and mix by the weight percent of total reaction material, 80 ℃ of temperature of reaction, reaction times is no less than 16 hours, and reaction generates modified calcium aluminate.
Embodiment 3, the aqueous solution, tensio-active agent metatitanic acid fat consumption that with primary industry lime and aluminium hydroxide by the mol ratio of calcium and aluminium are 1.80: 1.00 are 2.60 to drop in the reactors and mix by the weight percent of total reaction material, 120 ℃ of temperature of reaction, reaction times is no less than 12 hours, and reaction generates modified calcium aluminate.
Embodiment 4, the aqueous solution, tensio-active agent zirconium aluminate consumption that with raw material milk of lime and aluminium hydroxide by the mol ratio of calcium and aluminium are 2.40: 1.00 are 2.00 to drop in the reactors and mix by the weight percent of total reaction material, 65 ℃ of temperature of reaction, reaction times is no less than 14 hours, and reaction generates modified calcium aluminate.
The additive that the modified calcium aluminate that above embodiment generated can directly be made coating uses, also can get finished product after filtering, but for the ease of using, the calcium aluminate after the filtration again after drying, pulverizing, the packing so that transportation, and filtrate filtered adds and continues in the reactor to use.Technology of the present invention is shown in the process flow diagram of accompanying drawing 1.
Compare with calcium aluminate international standard x optical diffraction data (seeing attached list shown in 3) by the x optical diffraction data (seeing attached list shown in 2) to embodiment 4 products obtained therefroms, the main peak Value Data is all identical substantially.
Be the application testing comparison of the modified calcium aluminate produced with the present invention below: with paste PVC (polyvinyl chloride) 100phr(part with lime carbonate, aluminium hydroxide, general calcium aluminate), DOP(phthalic acid di-isooctyl) 65phr(part) stablizer (three salt) 5phr(part), each material of additive (variable) stirs, put into mould, 185～190 ℃ of plasticizings 5 minutes, make thick 1 millimeter matrix, wherein additive can be modified calcium aluminate and lime carbonate, aluminium hydroxide, general calcium aluminate;
A. the test of flame retardant resistance: oxygen determination index, subordinate list 4 are PVC diaphragm-operated oxygen index data under the different additions of different additive:
Learnt that by table 4 data the flame retardant properties of modified calcium aluminate is better than lime carbonate, a little more than aluminium hydroxide and general calcium aluminate, and along with the increase of modified calcium aluminate amount of filling, oxygen index is also along with growth.
B. absorb the ability of HCL, test HCL generating capacity, subordinate list 5 are PVC diaphragm-operated HCL generating capacity under the different additions of different additive:
Learn that by table 5 data the absorption HCL ability of modified calcium aluminate is better than aluminium hydroxide and general calcium aluminate, slightly is inferior to lime carbonate, and along with the increase of modified calcium aluminate amount of filling, the HCL generating capacity reduces.
C. smoke elimination property, subordinate list 6 is PVC diaphragm-operated smoke density data under the 30phr for different additive in amount of filling;
Learn that by table 6 data the smoke elimination of modified calcium aluminate is better than aluminium hydroxide, lime carbonate and general calcium aluminate.
D. to effects of tensile strength, subordinate list 7 is PVC diaphragm-operated tensile strength under the 30phr for different additive in amount of filling:
Learn that by table 7 data general calcium aluminate is close to goods effects of tensile strength and aluminium hydroxide, but greater than lime carbonate, the calcium aluminate of modification reduces significantly then to the detrimentally affect of the disconnected elongation of goods tension by contrast.
The present invention has short, technology characteristic of simple of reaction times, and because of product do not need the washing, thereby avoided pollution and the recovery problem thereof of washings to environment, and the calcium aluminate after the modification reduces greatly to the detrimentally affect of products machinery performance, its flame retardant properties, HCL receptivity, smoke elimination all are better than aluminium hydroxide and general calcium aluminate, and decomposition temperature is more than 250 ℃, be higher than aluminium hydroxide 205 ℃ of decomposition, therefore have Application Areas widely than aluminium hydroxide, the smoke resistance flame resistance that is particularly useful for the special plastics of some high processing temperatures is handled.
Table 2
dA Ⅰ/Ⅰ1 dA Ⅰ/Ⅰ1 dA Ⅰ/Ⅰ1 dA Ⅰ/Ⅰ1 dA Ⅰ/Ⅰ1
5.06 90 3.08 70 2.53 60 2.01 100 1.73 70
4.37 70 2.77 90 2.48 70 1.97 30 1.71 60
3.31 70 2.69 20 2.26 100 1.81 40 1.66 80
Table 3
dA Ⅰ/Ⅰ1 dA Ⅰ/Ⅰ1 dA Ⅰ/Ⅰ1 dA Ⅰ/Ⅰ1 dA Ⅰ/Ⅰ1
5.14 90 3.13 70 2.56 60 2.21 20 1.809 40
4.43 70 2.80 90 2.45 70 2.03 100 1.738 70
3.36 70 2.671 20 2.28 100 1.98 30 1.705 60
Table 4
Addition phr
Oxygen index 10.0 20.0 30.0 40.0
Fire retardant
Lime carbonate 24.4 23.5 23.0 can not become to mould
Aluminium hydroxide 24.0 25.0 26.0 26.5
Modified calcium aluminate 25.0 25.5 26.5 27.0
General calcium aluminate 24.5 25.0 26.0 26.5
Table 5
Addition phr
HCL generating capacity mg/g sample 10.0 20.0 30.0 40.0
Fire retardant
Lime carbonate 180.600 150.880 154.930 can not become to mould
Aluminium hydroxide 245.056 246.055 243.950-
Modified calcium aluminate 205.340 186.300 188.000 150.800
General calcium aluminate 220.100 200.900 195.600 160.200
Table 6
The general calcium aluminate of fire retardant lime carbonate aluminium hydroxide modified calcium aluminate
Smoke density mg/g sample 413.02 326.14 307.08 310.06
Table 7
The SiO that fire retardant lime carbonate aluminium hydroxide is general changes aluminic acid lipoprotein and changes titanic acid ester and change
Calcium aluminate calcium aluminate calcium aluminate calcium aluminate
Break tensile strength N/mm 4.78 4.29 4.36 4.69 5.00 6.00
Elongation rate of tensile failure % 152.0 136.7 130.0 166.7 183.3 212.9
Claims (3)
1, a kind of production method of modified calcium aluminate, to it is characterized in that raw material calcium oxide and aluminium hydroxide be 1.00～2.50 the aqueous solution, aluminic acid ester or titanic acid ester or zirconium aluminate consumption by the weight percent of total reaction material by the mol ratio of calcium and aluminium is 0.5～3.0 to drop in the reactor and mix, be not less than 60 ℃ in temperature of reaction, reaction times is no less than 10 hours, reaction generates modified calcium aluminate, then the calcium aluminate that generates is obtained finished product after filtration and after the drying.
2, modified calcium aluminate production method according to claim 1 is characterized in that filtrate filtered adds continuation use in the reactor again.
3, modified calcium aluminate production method according to claim 1 is characterized in that the raw material calcium oxide can be unslaked lime, acetylene slag, industrial lime, and raw aluminum hydroxide can be industrial aluminium hydroxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN92112151.2A CN1030138C (en) | 1992-09-22 | 1992-09-22 | Preparation method of modified calcium aluminate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN92112151.2A CN1030138C (en) | 1992-09-22 | 1992-09-22 | Preparation method of modified calcium aluminate |
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| Publication Number | Publication Date |
|---|---|
| CN1074196A CN1074196A (en) | 1993-07-14 |
| CN1030138C true CN1030138C (en) | 1995-10-25 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN92112151.2A Expired - Fee Related CN1030138C (en) | 1992-09-22 | 1992-09-22 | Preparation method of modified calcium aluminate |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1331752C (en) * | 2005-04-05 | 2007-08-15 | 郑州登峰熔料有限公司 | Production method of high-calcium type calcium aluminate |
| CN1331753C (en) * | 2005-09-14 | 2007-08-15 | 郑州登峰熔料有限公司 | Lightweight high-calcium type calcium aluminate production method |
| CN100430320C (en) * | 2005-12-22 | 2008-11-05 | 宝山钢铁股份有限公司 | Artificial synthesizing process for calcium aluminate |
| CN101077784B (en) * | 2006-05-26 | 2011-01-26 | 中国科学院金属研究所 | Nano CaAl4O7 material and preparing method thereof |
| CN103708513A (en) * | 2013-09-02 | 2014-04-09 | 常州市清流水处理剂有限公司 | High purity composite alumina powder for water treatment agent |
| CN107311209B (en) * | 2017-07-06 | 2018-07-13 | 西安建筑科技大学 | A kind of carbon/calcium aluminate composite powder and preparation method thereof |
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