CN108865264A - A kind of preparation method of quaternary ammonium salt-modified chlorinated paraffin - Google Patents
A kind of preparation method of quaternary ammonium salt-modified chlorinated paraffin Download PDFInfo
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- CN108865264A CN108865264A CN201810718292.0A CN201810718292A CN108865264A CN 108865264 A CN108865264 A CN 108865264A CN 201810718292 A CN201810718292 A CN 201810718292A CN 108865264 A CN108865264 A CN 108865264A
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G73/00—Recovery or refining of mineral waxes, e.g. montan wax
- C10G73/38—Chemical modification of petroleum
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Abstract
The invention discloses a kind of preparation methods of quaternary ammonium salt-modified chlorinated paraffin, chlorinated paraffin 70 is prepared using 2 footworks, pretreatment chlorinated paraffin is promoted further to react for chlorinated paraffin 70 under initiator effect, heat-resisting ester amine is introduced during the reaction, pass through the quaternization reaction of ester amine and dimethyl carbonate, realize the modification to chlorinated paraffin 70, the present invention prepares chlorinated paraffin 70 using Aqueous phase, various modifications are used during the preparation process, improve biocidal property, heat-resistant stability of finished product chlorinated paraffin material etc..
Description
Technical field
The invention belongs to chlorinated paraffin fields, and in particular to a kind of preparation method of quaternary ammonium salt-modified chlorinated paraffin.
Background technique
Chlorinated paraffin has the characteristics that odorless, nontoxic, fire-retardant, volatility is low and good with polyvinyl chloride resin compatibility, frequently as
The plasticizer of polyvinyl chloride, rubber, coating, ink additive, be machined additive, the anti-coagulants of lubricating oil, and modeling
Material, fire retardant of rubber etc., chlorinated paraffin due to containing the unstable chlorine atom on a small amount of or micro tertiary carbon atom, when heated or
When solar radiation, such unstable chlorine atom voluntarily can be detached from carbochain with adjacent hydrogen atom simultaneously, release HCl, HCl is again
The decomposition of chlorinated paraffin can further be promoted；Therefore, color can gradually add when the chlorinated paraffin product resting period is too long or heated
It is deep, its use is influenced, the raw materials used purity of domestic chlorinated paraffin, chlorination process and equipment have one compared with foreign countries
Fixed gap, thus chlorinated paraffin thermal stability is poor, causes heat stabilizer additive amount larger, stabilizer expense accounts for chlorinated paraffin
The share of cost is higher, and therefore, one of purpose of the invention is exactly not use for chlorinated paraffin to be blended with heat-resisting stabilizing agent
The mode of storage improves the heat-resistant stability of chlorinated paraffin；
Chlorinated paraffin can react with metal surface generate layered crystal structure at relatively high temperatures as EP agent
Chloride extreme pressure film slow down the generation of built-up edge to prevent the increase for being detained substance on blade, reduce tool wear, drop
Low workpiece surface roughness, according to statistics, China Metalworking fluid market are 20,000 t/a or so to the demand of chlorinated paraffin, and are adopted
With chlorinated paraffin, treated that metalwork cleans difficulty, not only needs to consume a large amount of organic solvent, but also will cause environment
Pollution, therefore, another object of the present invention is to prepare water-soluble chlorinated paraffin, to expand the application model of traditional chlorinated paraffin
It encloses, is especially easily removed after being used as metal conditioner.
Summary of the invention
In view of the defects and deficiencies of the prior art, the present invention intends to provide a kind of quaternary ammonium salt-modified chlorinated paraffins
Preparation method.
To achieve the above object, the present invention uses following technical scheme：
A kind of preparation method of quaternary ammonium salt-modified chlorinated paraffin, includes the following steps：
(1) octylisothiazolinone for taking 1.8-2 parts by weight is added in the dimethyl carbonate of 10-17 times of its weight, stirs
It mixes uniformly, obtains bacteriostatic solution；
(2) the smart wax for taking 90-100 parts by weight, is added in above-mentioned bacteriostatic solution, stirs evenly, be sent in reaction kettle,
It is passed through chlorine, adjusting temperature of reaction kettle is 40-50 DEG C, is stirred to react to liquid specific gravity and reaches 1.37-1.50, and discharging cooling obtains
Pre-process paraffin solution；
(3) the stearic acid zinc soap for taking 0.8-1 parts by weight, is added in the dehydrated alcohol of 10-13 times of its weight, stirs molten
Solution, is added the triethanolamine of 10-12 parts by weight, and slowly increasing temperature is 50-55 DEG C, insulated and stirred 20-40 minutes, is distilled off
Ethyl alcohol obtains heat resistance modified triethanolamine；
(4) above-mentioned heat resistance modified triethanolamine is taken, mixes, stirs evenly with the stearic acid of 13-20 parts by weight, is sent to anti-
It answers in kettle, is added to the p-methyl benzenesulfonic acid of mixture weight 2-3%, be passed through nitrogen, adjusting temperature of reaction kettle is 150-180
DEG C, it is stirred to react 5-6 hours, is cooled to room temperature, discharging cooling obtains heat-resisting ester amine；
(5) surfactant for taking 0.8-1.5 parts by weight is added in the deionized water of 10-17 times of its weight, and stirring is equal
It is even, obtain aqueous dispersions；
(6) above-mentioned heat-resisting ester amine is taken, is added in pretreatment paraffin solution, is stirred evenly, be sent in reaction kettle, be passed through
Nitrogen, adjusting temperature of reaction kettle is 55-60 DEG C, reacts 30-40 hours, above-mentioned aqueous dispersions are added, stir evenly, are passed through chlorine
Gas, adjusting reactor pressure are 0.2-0.3Mpa, and the initiator of 0.1-0.2 parts by weight is added, and adjusting temperature of reaction kettle is 90-
It 110 DEG C, reacts 4-6 hours, discharging rotates 1-2 hours at 93-95 DEG C, filters, filter cake is washed with lye, air drying, i.e.,
?.
The surfactant is one of Dodecydimethylammonium bronides, neopelex.
The initiator is ammonium persulfate.
The lye is the sodium hydroxide solution that concentration is 0.1-0.2mol/l.
Advantages of the present invention：
The present invention, using the dimethyl carbonate solution of octylisothiazolinone as reaction solution, passes through chlorine using smart wax as raw material
Solid/liquid/gas reactions obtain pretreated chlorinated paraffin, handle triethanolamine using stearic acid zinc soap later, and stearic acid blending reaction,
Heat resistance modified ester amine is obtained, promotes pretreatment chlorinated paraffin further to react for chlorinated paraffin under initiator effect later
70, heat-resisting ester amine is introduced during the reaction, by the quaternization reaction of ester amine and dimethyl carbonate, is realized to chlorinated paraffin
70 modification, the present invention prepare chlorinated paraffin 70 using Aqueous phase, use various modifications during the preparation process, improve into
Biocidal property, the heat-resistant stability etc. of product chlorinated paraffin material, modification through the invention, obtained finished-product material storage are steady
It is qualitative good, because quaternary ammonium salt-modified, it can be distributed in water when in use, good dispersion, improve traditional chlorinated paraffin 70
Characteristic not soluble in water, traditional chlorinated paraffin 70 is only used as fire retardant mostly and uses, and modification through the invention, enriches
Its effect, expands its use scope, and can distribute it in water and use, the feature of environmental protection is good, and finished product of the invention may be used also
To be widely used in punching press, stretching, drawing, the cutting of the various metals such as stainless steel, high lubricating effect is directly rushed with water after use
It washes, cleaning can be completed, do not need a large amount of organic solvent not only, economize on resources, and is i.e. convenient and environmentally friendly.
Specific embodiment
Embodiment 1
A kind of preparation method of quaternary ammonium salt-modified chlorinated paraffin, includes the following steps：
(1) octylisothiazolinone for taking 1.8 parts by weight is added in the dimethyl carbonate of 10 times of its weight, and stirring is equal
It is even, obtain bacteriostatic solution；
(2) the smart wax for taking 90 parts by weight, is added in above-mentioned bacteriostatic solution, stirs evenly, be sent in reaction kettle, be passed through
Chlorine, adjusting temperature of reaction kettle is 40 DEG C, is stirred to react to liquid specific gravity and reaches 1.37, and it is molten must to pre-process paraffin for discharging cooling
Liquid；
(3) the stearic acid zinc soap for taking 0.8 parts by weight is added in the dehydrated alcohol of 10 times of its weight, stirring and dissolving, is added
The triethanolamine of 10 parts by weight, slowly increasing temperature is 50 DEG C, and insulated and stirred 20-40 minutes, ethyl alcohol is distilled off, obtains heat-resisting change
Property triethanolamine；
(4) above-mentioned heat resistance modified triethanolamine is taken, mixes, stirs evenly with the stearic acid of 13 parts by weight, is sent to reaction
In kettle, it is added to the p-methyl benzenesulfonic acid of mixture weight 2%, is passed through nitrogen, adjusting temperature of reaction kettle is 170 DEG C, and stirring is anti-
It answers 6 hours, is cooled to room temperature, discharging cooling obtains heat-resisting ester amine；
(5) Dodecydimethylammonium bronides for taking 0.8 parts by weight are added in the deionized water of its weight 10, stirring
Uniformly, aqueous dispersions are obtained；
(6) above-mentioned heat-resisting ester amine is taken, is added in pretreatment paraffin solution, is stirred evenly, be sent in reaction kettle, be passed through
Nitrogen, adjusting temperature of reaction kettle is 55 DEG C, reacts 30 hours, above-mentioned aqueous dispersions are added, stir evenly, are passed through chlorine, is adjusted
Reactor pressure is 0.2Mpa, and the ammonium persulfate of 0.1 parts by weight is added, and adjusting temperature of reaction kettle is 90 DEG C, reaction 4 hours, out
Material, rotate 1 hour at 93 DEG C, suction filtration, filter cake is washed with lye, air drying to get.
The lye is the sodium hydroxide solution that concentration is 0.1mol/l.
Embodiment 2
A kind of preparation method of quaternary ammonium salt-modified chlorinated paraffin, includes the following steps：
(1) octylisothiazolinone for taking 2 parts by weight is added in the dimethyl carbonate of 17 times of its weight, stirs evenly,
Obtain bacteriostatic solution；
(2) the smart wax for taking 100 parts by weight, is added in above-mentioned bacteriostatic solution, stirs evenly, be sent in reaction kettle, leads to
Enter chlorine, adjusting temperature of reaction kettle is 50 DEG C, is stirred to react to liquid specific gravity and reaches 1.48, and discharging cooling obtains pretreatment paraffin
Solution；
(3) the stearic acid zinc soap for taking 1 parts by weight is added in the dehydrated alcohol of 13 times of its weight, stirring and dissolving, is added 12
The triethanolamine of parts by weight, slowly increasing temperature is 55 DEG C, and insulated and stirred 20-40 minutes, ethyl alcohol is distilled off, obtains heat resistance modified
Triethanolamine；
(4) above-mentioned heat resistance modified triethanolamine is taken, mixes, stirs evenly with the stearic acid of 20 parts by weight, is sent to reaction
In kettle, it is added to the p-methyl benzenesulfonic acid of mixture weight 3%, is passed through nitrogen, adjusting temperature of reaction kettle is 180 DEG C, and stirring is anti-
It answers 6 hours, is cooled to room temperature, discharging cooling obtains heat-resisting ester amine；
(5) neopelex for taking 1 parts by weight is added in the deionized water of 17 times of its weight, stirs evenly,
Obtain aqueous dispersions；
(6) above-mentioned heat-resisting ester amine is taken, is added in pretreatment paraffin solution, is stirred evenly, be sent in reaction kettle, be passed through
Nitrogen, adjusting temperature of reaction kettle is 60 DEG C, reacts 40 hours, above-mentioned aqueous dispersions are added, stir evenly, are passed through chlorine, is adjusted
Reactor pressure is 0.3Mpa, and the ammonium persulfate of 0.2 parts by weight is added, and adjusting temperature of reaction kettle is 110 DEG C, reaction 6 hours, out
Material, rotate 2 hours at 95 DEG C, suction filtration, filter cake is washed with lye, air drying to get.
The lye is the sodium hydroxide solution that concentration is 0.2mol/l.
Embodiment 3
A kind of preparation method of quaternary ammonium salt-modified chlorinated paraffin, includes the following steps：
(1) octylisothiazolinone for taking 1.9 parts by weight is added in the dimethyl carbonate of 12 times of its weight, and stirring is equal
It is even, obtain bacteriostatic solution；
(2) the smart wax for taking 95 parts by weight, is added in above-mentioned bacteriostatic solution, stirs evenly, be sent in reaction kettle, be passed through
Chlorine, adjusting temperature of reaction kettle is 43 DEG C, is stirred to react to liquid specific gravity and reaches 1.44, and it is molten must to pre-process paraffin for discharging cooling
Liquid；
(3) the stearic acid zinc soap for taking 0.9 parts by weight is added in the dehydrated alcohol of 12 times of its weight, stirring and dissolving, is added
The triethanolamine of 11 parts by weight, slowly increasing temperature is 52 DEG C, and insulated and stirred 23 minutes, ethyl alcohol is distilled off, obtains heat resistance modified
Triethanolamine；
(4) above-mentioned heat resistance modified triethanolamine is taken, mixes, stirs evenly with the stearic acid of 17 parts by weight, is sent to reaction
In kettle, it is added to the p-methyl benzenesulfonic acid of mixture weight 2%, is passed through nitrogen, adjusting temperature of reaction kettle is 173 DEG C, and stirring is anti-
It answers 6 hours, is cooled to room temperature, discharging cooling obtains heat-resisting ester amine；
(5) surfactant for taking 0.9 parts by weight is added in the deionized water of 12 times of its weight, stirs evenly, obtain water
Dispersion liquid；
(6) above-mentioned heat-resisting ester amine is taken, is added in pretreatment paraffin solution, is stirred evenly, be sent in reaction kettle, be passed through
Nitrogen, adjusting temperature of reaction kettle is 58 DEG C, reacts 32 hours, above-mentioned aqueous dispersions are added, stir evenly, are passed through chlorine, is adjusted
Reactor pressure is 0.23Mpa, and the initiator of 0.13 parts by weight is added, and adjusting temperature of reaction kettle is 95 DEG C, reaction 5 hours, out
Material, rotate 1 hour at 93 DEG C, suction filtration, filter cake is washed with lye, air drying to get.
The surfactant is Dodecydimethylammonium bronides.
The initiator is ammonium persulfate.
The lye is the sodium hydroxide solution that concentration is 0.14mol/l.
Performance test：
By the comparison of the quaternary ammonium salt-modified chlorinated paraffin of the embodiment of the present invention 1,2,3 and commercially available chlorinated paraffin 70 (comparative example)
Test data is as shown in the table：
The test experiments of the resistance to thermal decomposition temperature process that the present invention uses for：
1. instrument and test paper
(1) test tube：It is 12 ± 1 millimeters of internal diameter, 14 ± 1 millimeters of outer diameter, 95 ± 1 millimeters long.
(2) heat resistant glass cup：140 ± 5 millimeters of internal diameter, 150 ± 5 millimeters of outer diameter, 110 ± 5 millimeters high, top is with 5 millis
The thick asbestos lid of rice, has covered 4~6 symmetrical test tube holes, has been inserted with the hole of thermometer and blender respectively in intermediate appropriate location
Each one.
(3) thermometer：0-200 DEG C of scale, scale division value is 1 DEG C.
(4) electric mixer and attached speed control device.
(5) square position electric furnace：1000-1500 watts and attached pressure regulator.
(6) glycerol.
(7) Congored test paper.
2. determination step
In being put into 1 ± 0.1 gram of sample in test tube, a Congored test paper (edging), the Congo are embedded in the upper edge of pipe
Red test paper keeps 7 millimeters or so at test tube space, and clogs test tube mouth with rubber stopper, and test tube is put into glycerol bath, makes to try
14 millimeters of (exposed portion) is covered away from bath in pipe top, and about 50 millimeters of glycerin liquid identity distance test tube top edge.It is inserted into chronothermometer
It is bordering on oil bath center appropriate location, makes mercury ball center and sample in same level, heats oil bath, and be stirred continuously, is heated up
Speed is no more than 4 DEG C per minute, when 30 DEG C before near-thermal decomposition temperature waiting, is heated up per minute with 2 DEG C, when Congored test paper is following
When blue is presented, temperature at this time, the as thermal decomposition temperature of sample are recorded.
3. precision
Difference is not more than 2 DEG C between parallel determinations, using the arithmetic mean of instantaneous value of parallel determinations as the heat of sample point
Solve temperature.
Claims (4)
1. a kind of preparation method of quaternary ammonium salt-modified chlorinated paraffin, which is characterized in that include the following steps：
(1) octylisothiazolinone for taking 1.8-2 parts by weight is added in the dimethyl carbonate of 10-17 times of its weight, and stirring is equal
It is even, obtain bacteriostatic solution；
(2) the smart wax for taking 90-100 parts by weight, is added in above-mentioned bacteriostatic solution, stirs evenly, be sent in reaction kettle, be passed through
Chlorine, adjusting temperature of reaction kettle is 40-50 DEG C, is stirred to react to liquid specific gravity and reaches 1.37-1.50, and discharging cooling obtains pre- place
Fibrous gypsum wax solution；
(3) the stearic acid zinc soap for taking 0.8-1 parts by weight, is added in the dehydrated alcohol of 10-13 times of its weight, and stirring and dissolving adds
Enter the triethanolamine of 10-12 parts by weight, slowly increasing temperature is 50-55 DEG C, insulated and stirred 20-40 minutes, ethyl alcohol is distilled off,
Obtain heat resistance modified triethanolamine；
(4) above-mentioned heat resistance modified triethanolamine is taken, mixes, stirs evenly with the stearic acid of 13-20 parts by weight, be sent to reaction kettle
In, the p-methyl benzenesulfonic acid of mixture weight 2-3% is added, is passed through nitrogen, adjusting temperature of reaction kettle is 150-180 DEG C, stirring
Reaction 5-6 hours, is cooled to room temperature, and discharging cooling obtains heat-resisting ester amine；
(5) surfactant for taking 0.8-1.5 parts by weight is added in the deionized water of 10-17 times of its weight, stirs evenly,
Obtain aqueous dispersions；
(6) above-mentioned heat-resisting ester amine is taken, is added in pretreatment paraffin solution, is stirred evenly, be sent in reaction kettle, be passed through nitrogen
Gas, adjusting temperature of reaction kettle is 55-60 DEG C, reacts 30-40 hours, above-mentioned aqueous dispersions are added, stir evenly, are passed through chlorine,
Adjusting reactor pressure is 0.2-0.3Mpa, and the initiator of 0.1-0.2 parts by weight is added, and adjusting temperature of reaction kettle is 90-110
DEG C, react 4-6 hour, discharging, rotated 1-2 hours at 93-95 DEG C, suction filtration, filter cake is washed with lye, air drying to get.
2. a kind of preparation method of quaternary ammonium salt-modified chlorinated paraffin according to claim 1, which is characterized in that the table
Face activating agent is one of Dodecydimethylammonium bronides, neopelex.
3. a kind of preparation method of quaternary ammonium salt-modified chlorinated paraffin according to claim 1, which is characterized in that described draws
Hair agent is ammonium persulfate.
4. a kind of preparation method of quaternary ammonium salt-modified chlorinated paraffin according to claim 1, which is characterized in that the alkali
Liquid is the sodium hydroxide solution that concentration is 0.1-0.2mol/l.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109535827A (en) * | 2018-12-28 | 2019-03-29 | 张展清 | A kind of corrosion-resistanting ink and preparation method thereof |
| CN110511576A (en) * | 2019-07-23 | 2019-11-29 | 肥东县云武研发有限公司 | A kind of glass lost-wax process casting paraffin and preparation method thereof |
| CN112647286A (en) * | 2019-11-03 | 2021-04-13 | 苏州新而特纺织有限公司 | Textile dye |
| CN114797513A (en) * | 2022-04-11 | 2022-07-29 | 云南磷化集团有限公司 | Preparation method of label protective film for laboratory reagent bottle |
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| CN110511576A (en) * | 2019-07-23 | 2019-11-29 | 肥东县云武研发有限公司 | A kind of glass lost-wax process casting paraffin and preparation method thereof |
| CN112647286A (en) * | 2019-11-03 | 2021-04-13 | 苏州新而特纺织有限公司 | Textile dye |
| CN114797513A (en) * | 2022-04-11 | 2022-07-29 | 云南磷化集团有限公司 | Preparation method of label protective film for laboratory reagent bottle |
| CN114797513B (en) * | 2022-04-11 | 2024-01-26 | 云南磷化集团有限公司 | Preparation method of label protection film of laboratory reagent bottle |
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Address after: 237451 Huhu Town, Huoqiu County, Lu'an City, Anhui Province Patentee after: Anhui Xingxin Material Technology Co.,Ltd. Address before: 237451 Huhu Town, Huoqiu County, Lu'an City, Anhui Province Patentee before: ANHUI XINGXIN CHEMICAL TECHNOLOGY Co.,Ltd. |