CN106011907B - A kind of tetrachloro-ethylene stabilizer and preparation method thereof - Google Patents
A kind of tetrachloro-ethylene stabilizer and preparation method thereof Download PDFInfo
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- CN106011907B CN106011907B CN201610389109.8A CN201610389109A CN106011907B CN 106011907 B CN106011907 B CN 106011907B CN 201610389109 A CN201610389109 A CN 201610389109A CN 106011907 B CN106011907 B CN 106011907B
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G5/00—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents
- C23G5/02—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents using organic solvents
- C23G5/028—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents using organic solvents containing halogenated hydrocarbons
- C23G5/02854—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents using organic solvents containing halogenated hydrocarbons characterised by the stabilising or corrosion inhibiting additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
- C07C17/42—Use of additives, e.g. for stabilisation
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Abstract
The present invention provides a kind of tetrachloro-ethylene stabilizer, and the stabilizer includes following material composition：Triethanolamine, pentane, fourth chloropharin, butylene oxide, thymol.The present invention also provides the preparation methods of aforementioned stable agent.Stabilizer prepared by the present invention is applied in tetrachloro-ethylene production, and the quality index of tetrachloro-ethylene is after addition stabilizer：Purity 99.9615 99.9918%, pH be 9.62 9.75, moisture be 16 18ppm, colourity 10；After 360 days, the purity change rate of tetrachloro-ethylene is 0 0.038%, and pH change rates are 0.1 0.2%, and moisture and colourity are unchanged.Stabilizer prepared by the present invention, for tetrachloro-ethylene, service life was up to 2 years；Stabilizer prepared by the present invention, thermal stability is good, and anti-moisture performance is good, and cleaning equipment and workpiece will not be corroded.
Description
Technical field
The present invention relates to a kind of tetrachloro-ethylene stabilizer, specifically, be related to a kind of tetrachloro-ethylene stabilizer and its
Preparation method.
Background technology
Tetrachloro-ethylene have high-solvency, high osmosis, it is non-ignitable, non-corrosive, the excellent performances such as be easily recycled, widely
As dry cleaning fabric agent, metal degreasing agent and common solvent.
Tetrachloro-ethylene generally is produced on an industrial scale, in storage or effect, easy light, empty air and heat, moisture or metal
Surface etc. influences and decomposes, acidic materials or the tarry matters such as generation hydrochloric acid, phosgene, trichloroacetic acid.These decomposition products,
Pollution damage fiber, etching apparatus, corrode wash mill and metal product in degreasing metal washing in dry-cleaning.In order to prevent
Tetrachloro-ethylene decomposes, and need to add in stabilizer, it is ensured that product quality is stablized.
Existing tetrachloro-ethylene stabilizer, has the following disadvantages：
（1）For tetrachloro-ethylene, in 360 days, the mass change of tetrachloro-ethylene is big；
（2）Service life is short
（3）Thermal stability is poor, and anti-moisture performance is poor, high to the rate of corrosion of equipment.
The content of the invention
To solve the shortcomings of the prior art, the present invention provides a kind of tetrachloro-ethylene stabilizer and preparation method thereof,
To realize following goal of the invention：
（1）Stabilizer prepared by the present invention, for tetrachloro-ethylene, in 360 days, the purity of tetrachloro-ethylene is constant, acid value（With
HCL is counted）It is basically unchanged, pH value is basically unchanged, moisture is basically unchanged, colourity（Hazen unit platinum-cobalt colors number）It is basically unchanged；
（2）Stabilizer prepared by the present invention, for tetrachloro-ethylene, usage time is up to 2 years；
（3）Stabilizer prepared by the present invention, thermal stability is good, and anti-moisture performance is good, low to the rate of corrosion of equipment.
For solution more than technical problem, the technical solution that the present invention takes is as follows：
A kind of tetrachloro-ethylene stabilizer, it is characterised in that：The stabilizer includes following material composition：
Triethanolamine, pentane, fourth chloropharin, butylene oxide, thymol.
It is that above-mentioned technical proposal is further improved below：
The stabilizer includes the component of following parts by weight：
50-100 parts of triethanolamine, 50-100 parts of n-amyl alcohol, 50-100 parts of fourth chloropharin, 50-100 parts of butylene oxide, Moschus
Careless phenol 5-10 parts.
Further, the stabilizer includes the component of following parts by weight：
58-70 parts of triethanolamine, 50-100 parts of n-amyl alcohol, 50-100 parts of fourth chloropharin, 50-100 parts of butylene oxide, thyme
5 parts of phenol.
Further, the stabilizer includes the component of following parts by weight：
60-64 parts of triethanolamine, 55-80 parts of n-amyl alcohol, 55-75 parts of fourth chloropharin, 52-80 parts of butylene oxide, thymol 5
Part.
Further, the stabilizer includes the component of following parts by weight：
65-70 parts of triethanolamine, 82-95 parts of n-amyl alcohol, 76-100 parts of fourth chloropharin, 82-100 parts of butylene oxide, thyme
5 parts of phenol.
The stabilizer, the dosage in tetrachloro-ethylene are 0.0205-0.041wt%.
The stabilizer, the dosage in tetrachloro-ethylene are preferably 0.0213-0.0375wt%.
The triethanolamine, product hierarchy are I types, triethanolamine purity >=99 wt%, 0.20 wt% of water content ＜, color
Degree≤50.
The pentane, purity >=99.5 wt%, 0.05 wt% of moisture content ＜, colourity≤20.
The fourth chloropharin, purity >=98wt%, chloride content ＜ 0.001wt%, water content ＜ 0.025wt%, colourity≤
15；The butylene oxide, purity >=99wt%, moisture content ＜ 0.020wt%, colourity≤10；The thymol, content >=99wt%,
Appearance is white crystalline body.
The tetrachloro-ethylene, tetrachloro-ethylene purity >=99.99wt%；In terms of HCL, tetrachloro-ethylene acid value≤10ppm；Tetrachloro
Ethylene moisture≤30ppm；Tetrachloro-ethylene colourity≤10；The tetrachloro-ethylene, after adding in stabilizer, pH value 9.5-10.
A kind of preparation method of tetrachloro-ethylene stabilizer, each ingredient is taken according to the parts by weight, in normal temperature and pressure, closing
Under the conditions of, it by ingredient stirring, is uniformly mixed, obtains stabilizer.
Compared with prior art, beneficial effects of the present invention are：
（1）Stabilizer prepared by the present invention is applied in tetrachloro-ethylene production, the result feedback that tracking product quality obtains
Well, the quality index of tetrachloro-ethylene is after addition stabilizer：Purity 99.9615-99.9918%, pH 9.62-9.75, moisture
Content is 16-18ppm, colourity 10；After 360 days, the quality index of tetrachloro-ethylene is：Purity 99.9615-99.9701%, pH
For 9.60-9.71, moisture 16-18ppm, colourity 10；360 days, the purity change rate of tetrachloro-ethylene was 0-0.038%,
PH change rates are 0.1-0.2%, and moisture and colourity are unchanged；
（2）Stabilizer prepared by the present invention, for tetrachloro-ethylene, service life 2 years；
（3）Stabilizer prepared by the present invention, thermal stability is good, and anti-moisture performance is good, and will not be to cleaning equipment and work
Part corrodes, and illustrates this cleaning field for being applied to precision metallic part to tetrachloro-ethylene, so as to four chloroethene of import outside surrogate
Alkene has very important significance；
The result of copper strip test：After stabilizer prepared by the present invention is used for tetrachloro-ethylene, copper strip test is carried out,
Copper corrosion amount is 0.014-0.016mg/m2, tetrachloro-ethylene solution colour is：It is almost colourless, before the pH of tetrachloro-ethylene is by testing
9.62-9.75, for 9.21-9.39 after experiment, pH change rates are 3.69-4.26%；
Control group, carries out copper strip test, and copper corrosion amount is 0.020mg/m2, tetrachloro-ethylene solution colour is：It is shallow
Yellow, the pH of tetrachloro-ethylene are that 8.16, pH change rates are 13.83% after experiment by 9.47 before testing.
Specific embodiment
The preferred embodiment of the present invention is illustrated below, it should be appreciated that preferred embodiment described herein is only used
In the description and interpretation present invention, it is not intended to limit the present invention.
A kind of 1 tetrachloro-ethylene stabilizer of embodiment
Include the component of following parts by weight：
Triethanolamine 58g, 50 g of pentane, 50 g of fourth chloropharin, 50 g of butylene oxide, 5 g of thymol,
Dosage of the stabilizer in tetrachloro-ethylene is 0.0213%；
The triethanolamine is produced by Laiyang economic and technological development zone Fine Chemical Works.
The pentane is produced by Shanghai Ling Feng chemical reagent Co., Ltd.
The thymol is produced by Tianjin City Chemical Agent Research Institute.
The butylene oxide is by Japanese imported with original packaging product.
The fourth chloropharin is by Japanese imported with original packaging product.
The quality requirement of each ingredient in stabilizer of the present invention：
1 triethanolamine quality index of table
2 pentane quality index of table
3 fourth chloropharin quality index of table
4 butylene oxide quality index of table
5 thymol quality index of table
The tetrachloro-ethylene that tetrachloro-ethylene stabilizer of the present invention is applicable in has claimed below：
Raw material tetrachloro-ethylene purity >=99.99%；
Raw material tetrachloro-ethylene acid value（In terms of HCL）≤10ppm；
Raw material tetrachloro-ethylene moisture≤30ppm；
Raw material tetrachloro-ethylene colourity（Hazen unit platinum-cobalt colors number）≤10.
Stabilizer described in embodiment 1, for tetrachloro-ethylene produce in, analysis detection add in stabilizer after initial mass with
And the quality in 360 days, it is shown in Table 6.
The stabilizing effect of stabilizer described in 6 embodiment 1 of table
In addition after stabilizer of the present invention is used for tetrachloro-ethylene, service life 2 years；
Copper corrosion is tested：
Of the present invention group：Add in the tetrachloro-ethylene of stabilizer described in embodiment 1；
Control：Select import tetrachloro-ethylene material as a comparison.
Experimental method：
Two pieces of 50mm × 2.5mm × 0.05mm of preparation, the electrolytic copper foil of purity more than 99.9%, after hydrochloric acid, water washing,
It dries, 30min is dried in 105 ± 2 DEG C of baking ovens, is weighed spare.
Tetrachloro-ethylene sample 135ml, water 5ml are put into spherical fat extractor displacer, one piece of copper sheet is placed in extractor,
Another piece is hung in condenser lower end with line.Circulation is heated, every 8 ~ 10 minutes circulation once.Circulation for a period of time after, stop plus
Heat takes out copper sheet, weighs after pickling, washing, drying, the sum of etching extent of two pieces of copper sheets is obtained, according to the size of etching extent
It determines the stablizing effect of stabilizer, and observes the color of tetrachloro-ethylene solution, detect pH value, be specifically shown in Table 7.
Table 7 adds in the performance test of the tetrachloro-ethylene of stabilizer described in embodiment 1：
A kind of 2 tetrachloro-ethylene stabilizer of embodiment
Include the component of following parts by weight：Triethanolamine 64g, 80 g of pentane, 80 g of fourth chloropharin, 80 g of butylene oxide,
5 g of thymol；
Dosage of the stabilizer in tetrachloro-ethylene is 0.0309%；
The triethanolamine is produced by Laiyang economic and technological development zone Fine Chemical Works.
The pentane is produced by Shanghai Ling Feng chemical reagent Co., Ltd.
The thymol is produced by Tianjin City Chemical Agent Research Institute.
The butylene oxide is by Japanese imported with original packaging product.
The fourth chloropharin is by Japanese imported with original packaging product.
Requirement of the tetrachloro-ethylene stabilizer of the present invention to tetrachloro-ethylene：
Raw material tetrachloro-ethylene purity >=99.99%；
Raw material tetrachloro-ethylene acid value（In terms of HCL）≤10ppm；
Raw material tetrachloro-ethylene moisture≤30ppm；
Raw material tetrachloro-ethylene colourity（Hazen unit platinum-cobalt colors number）≤10.
The quality requirement of each ingredient in the present embodiment stabilizer, with embodiment 1.
Stabilizer described in embodiment 2, for tetrachloro-ethylene produce in, analysis detection add in stabilizer after initial mass with
And the quality in 360 days, it is shown in Table 8.
The stabilizing effect of stabilizer described in 8 embodiment 2 of table
After stabilizer of the present invention is used for tetrachloro-ethylene, service life 2 years；
It is tested using the copper corrosion described in embodiment 1, the results are shown in Table 9：
Table 9 adds in the tetrachloro-ethylene performance test of stabilizer described in embodiment 2：
A kind of 3 tetrachloro-ethylene stabilizer of embodiment
Include the component of following parts by weight：Triethanolamine 70g, 100 g of pentane, 100 g of fourth chloropharin, butylene oxide 100
G, 5 g of thymol；
Dosage of the stabilizer in tetrachloro-ethylene is 0.0375%；
The triethanolamine is produced by Laiyang economic and technological development zone Fine Chemical Works.
The pentane is produced by Shanghai Ling Feng chemical reagent Co., Ltd.
The thymol is produced by Tianjin City Chemical Agent Research Institute.
The butylene oxide is by Japanese imported with original packaging product.
The fourth chloropharin is by Japanese imported with original packaging product.
Requirement of the tetrachloro-ethylene stabilizer of the present invention to tetrachloro-ethylene：
Raw material tetrachloro-ethylene purity >=99.99%；
Raw material tetrachloro-ethylene acid value（In terms of HCL）≤10ppm；
Raw material tetrachloro-ethylene moisture≤30ppm；
Raw material tetrachloro-ethylene colourity（Hazen unit platinum-cobalt colors number）≤10.
The quality requirement of each ingredient in the present embodiment stabilizer, with embodiment 1.
Stabilizer described in embodiment 3, for tetrachloro-ethylene produce in, analysis detection add in stabilizer after initial mass with
And the quality in 360 days, it is shown in Table 10.
The stabilizing effect of stabilizer described in 10 embodiment 3 of table
After stabilizer of the present invention is used for tetrachloro-ethylene, service life 2 years；
It is tested using the copper corrosion described in embodiment 1, the results are shown in Table 11：
Table 11 adds in the tetrachloro-ethylene performance test of stabilizer described in embodiment 3：
A kind of preparation method of 4 tetrachloro-ethylene stabilizer of embodiment
（1）It weighs
According to the formula of stabilizer, each component is weighed；
（2）The mixing of pentane and fourth chloropharin
Load weighted pentane and fourth chloropharin are sealed into stirring at normal temperatures and pressures；
（3）Thymol and butylene oxide mixing
Load weighted drug thymol is added in butylene oxide solution, stirring is sealed under normal temperature and pressure, until musk deer
Vanilla phenol powder is dissolved completely in butylene oxide solution；
（4）Four kinds of component mixing
The mixed liquor of thymol and butylene oxide is added in the mixed liquor of pentane and fourth chloropharin, under normal temperature and pressure
Sealing stirs evenly；
（5）Add in triethanolamine
Triethanolamine is eventually adding, is stirred evenly, obtains stabilizer of the present invention.
A kind of application method of 5 tetrachloro-ethylene stabilizer of embodiment
When modulating finished product tetrachloro-ethylene, by stabilizer of the present invention according to the amount of 0.0213-0.0375%, tetrachloro is added to
In ethylene finished pot, open forced circulation pump and carry out Matter Transfer, so as to achieve the purpose that stabilizer is uniformly spread in material.
Finally it should be noted that：The foregoing is only a preferred embodiment of the present invention, is not intended to limit the invention,
Although the present invention is described in detail with reference to the foregoing embodiments, for those skilled in the art, still may be used
To modify to the technical solution recorded in foregoing embodiments or carry out equivalent substitution to which part technical characteristic.
Within the spirit and principles of the invention, any modifications, equivalent replacements and improvements are made should be included in the present invention's
Within protection domain.
Claims (8)
1. a kind of tetrachloro-ethylene stabilizer, it is characterised in that：The stabilizer includes following material composition：
Triethanolamine, pentane, fourth chloropharin, butylene oxide, thymol；
The stabilizer includes the component of following parts by weight：
50-100 parts of triethanolamine, 50-100 parts of n-amyl alcohol, 50-100 parts of fourth chloropharin, 50-100 parts of butylene oxide, thymol
5-10 parts；
The stabilizer, the dosage in tetrachloro-ethylene are 0.0205-0.041wt%.
2. a kind of tetrachloro-ethylene stabilizer according to claim 1, it is characterised in that：The stabilizer includes following heavy
Measure the component of part：
58-70 parts of triethanolamine, 50-100 parts of n-amyl alcohol, 50-100 parts of fourth chloropharin, 50-100 parts of butylene oxide, thymol 5
Part.
3. a kind of tetrachloro-ethylene stabilizer according to claim 1, it is characterised in that：The stabilizer, in four chloroethenes
Dosage in alkene is 0.0213-0.0375wt%.
4. a kind of tetrachloro-ethylene stabilizer according to claim 1, it is characterised in that：The triethanolamine, product etc.
Grade is I type, triethanolamine purity >=99 wt%, 0.20 wt% of water content ＜, colourity≤50.
5. a kind of tetrachloro-ethylene stabilizer according to claim 1, it is characterised in that：The pentane, purity >=
0.05 wt% of 99.5 wt%, moisture content ＜, colourity≤20.
6. a kind of tetrachloro-ethylene stabilizer according to claim 1, it is characterised in that：The fourth chloropharin, purity >=
98wt%, chloride content ＜ 0.001wt%, water content ＜ 0.025wt%, colourity≤15；The butylene oxide, purity >=
99wt%, moisture content ＜ 0.020wt%, colourity≤10；The thymol, content >=99wt%, appearance are white crystalline body.
7. a kind of tetrachloro-ethylene stabilizer according to claim 1, it is characterised in that：The tetrachloro-ethylene, four chloroethenes
Alkene purity >=99.99wt%；In terms of HCL, tetrachloro-ethylene acid value≤10ppm；Tetrachloro-ethylene moisture≤30ppm；Tetrachloro-ethylene colourity
≤10；The tetrachloro-ethylene, after adding in stabilizer, pH value 9.5-10.
8. a kind of preparation method of tetrachloro-ethylene stabilizer according to claim 1, it is characterised in that：According to described heavy
Amount part takes each ingredient, under normal temperature and pressure, sealing condition, by ingredient stirring, is uniformly mixed, obtains stabilizer.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111606779B (en) * | 2020-05-19 | 2022-09-30 | 国药集团化学试剂有限公司 | Tetrachloroethylene solid composite stabilizer and preparation method thereof |
| CN118239821A (en) * | 2024-03-22 | 2024-06-25 | 西陇科学股份有限公司 | Environment-friendly tetrachloroethylene and preparation method thereof |
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| CN102850179A (en) * | 2012-10-08 | 2013-01-02 | 江苏省格林艾普化工股份有限公司 | Stabilizer for trichloroethylene |
| CN103896723A (en) * | 2014-04-18 | 2014-07-02 | 山东新龙科技股份有限公司 | Stabilizer for trichloro ethylene and preparation method thereof |
| CN104072332A (en) * | 2013-03-27 | 2014-10-01 | 杭州泽泉生物科技有限公司 | Trichloroethylene stabilizing agent for cleaning |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0386838A (en) * | 1989-06-30 | 1991-04-11 | Asahi Glass Co Ltd | Method for stabilizing 1,1,2-trichloro-2,2-difluoroethane |
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| CN102850179A (en) * | 2012-10-08 | 2013-01-02 | 江苏省格林艾普化工股份有限公司 | Stabilizer for trichloroethylene |
| CN104072332A (en) * | 2013-03-27 | 2014-10-01 | 杭州泽泉生物科技有限公司 | Trichloroethylene stabilizing agent for cleaning |
| CN103896723A (en) * | 2014-04-18 | 2014-07-02 | 山东新龙科技股份有限公司 | Stabilizer for trichloro ethylene and preparation method thereof |
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| 《四氯乙烯稳定性研究》;潘懋;《氯碱工业》;19860630(第03期);第57-64页 * |
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