CN114369954B - Preparation method of anti-freezing emulsifier for spinning sizing - Google Patents

Preparation method of anti-freezing emulsifier for spinning sizing Download PDF

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Publication number
CN114369954B
CN114369954B CN202111654677.3A CN202111654677A CN114369954B CN 114369954 B CN114369954 B CN 114369954B CN 202111654677 A CN202111654677 A CN 202111654677A CN 114369954 B CN114369954 B CN 114369954B
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polyoxyethylene ether
emulsifier
fatty alcohol
spinning sizing
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CN114369954A (en
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沈亚芬
朱建成
陈小琴
朱通彧
仰国锋
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Tongxiang Henglong Chemical Co ltd
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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/53Polyethers
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/02Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with hydrocarbons
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/40Reduced friction resistance, lubricant properties; Sizing compositions

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
  • Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)

Abstract

The invention discloses a preparation method of an emulsifier for antifreeze spinning sizing, which comprises the following steps: 30-40 parts of self-made fatty alcohol polyoxyethylene ether by weight parts; 10 TO 15 portions of isomeric tridecanol polyoxyethylene ether TO-5 isomeric alcohol ether; 8-10 parts of multi-branched-chain isomeric tridecanol polyoxyethylene ether 1308; 10-20 parts of white oil; mixing to obtain the anti-freezing emulsifier for spinning sizing. The antifreeze type emulsifier for spinning sizing has the characteristics of difficult layering, antifreeze type and convenient subsequent use.

Description

Preparation method of anti-freezing emulsifier for spinning sizing
Technical Field
The invention relates to the technical field of spinning, in particular to a preparation method of an emulsifier for anti-freezing spinning sizing.
Background
Emulsifiers are substances which enable a mixed liquid of two or more components which are not compatible with each other to form a stable emulsion. The principle of action is that during emulsification, the dispersed phase is dispersed in the continuous phase in the form of droplets (micron-sized), the emulsifier reduces the interfacial tension of the components in the mixed system, and forms a stronger film on the surface of the droplets or an electric double layer on the surface of the droplets due to the charges given by the emulsifier, preventing the droplets from aggregating with each other, and maintaining a uniform emulsion. To express hydrophilicity or lipophilicity of an emulsifier, "hydrophilic-lipophilic balance (HLB value)", the lower the HLB value, the more lipophilic it is; conversely, the higher the HLB value, the more hydrophilic it is. The HLB values of the various emulsifiers vary, and in order to obtain a stable emulsion, the appropriate emulsifier must be selected.
The special emulsifying agent for spinning in the current market is generally a cationic surfactant, has weak hydrophilicity, is suitable for W/O type emulsion, has obvious limitation, is easy to layer and cannot realize the emulsifying effect rapidly when the external temperature is reduced, and has low efficiency.
Disclosure of Invention
The invention aims to solve the technical problems that: an anti-freezing type emulsifier for spinning sizing and a preparation method thereof are developed, and the anti-freezing type emulsifier for spinning sizing has the characteristics of difficult layering, anti-freezing type and convenient subsequent use.
The invention aims to solve the problems in the prior art and provides an anti-freezing emulsifier for spinning sizing and a preparation method thereof.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the preparation method of the antifreeze type emulsifier for spinning sizing comprises the following steps:
The components in parts by weight are as follows
30-40 Parts of self-made fatty alcohol polyoxyethylene ether;
10 TO 15 portions of isomeric tridecanol polyoxyethylene ether TO-5 isomeric alcohol ether;
8-10 parts of multi-branched-chain isomeric tridecanol polyoxyethylene ether 1308;
10-20 parts of white oil;
Mixing to obtain the anti-freezing emulsifier for spinning sizing.
As a further improvement of the scheme, the self-made fatty alcohol-polyoxyethylene ether is prepared by the following steps: the raw materials are the following raw materials in parts by weight
S1, sucking 180-220 parts of raw material C12-14 alcohol in an ethoxylation reaction device;
S2, adding 6-7.5 parts of alkali metal catalyst, dehydrating and circulating for more than 90 minutes at 120 ℃ by using a water ring vacuum pump, cooling to 80 ℃ for attempting to drop ethylene oxide, focusing on the temperature change of a heat exchanger of a reaction kettle at any time, controlling the temperature of a product in equipment to be 80+/-5 ℃, after 170-210 parts of ethylene oxide is dropped, preserving heat and curing, sampling and testing to be qualified, and cooling to 55 ℃ to obtain the fatty alcohol polyoxyethylene ether.
As a further improvement of this scheme, the alkali metal catalyst is KOH.
As a further improvement of the present scheme, the alkali metal catalyst is KOH, ca (NO 3)2.
As a further improvement of the scheme, the time of heat-preserving curing in S2 is at least 30min.
Compared with the prior art, the invention has the following beneficial effects:
The freezing-resistant emulsifier for spinning sizing is a nonionic emulsifier compounded by mixing fatty alcohol polyoxyethylene ether and white oil, and a product produced by low-temperature reaction has a more stable molecular structure, and ether bonds in the molecule are not easily damaged by acid and alkali, so that the emulsifier has the advantages of higher stability, good water solubility, electrolyte resistance, easiness in biodegradation and small foam, and simultaneously solves the problems that the traditional emulsifier is easy to generate layering and freezing in winter.
The self-made fatty alcohol polyvinyl ether and white oil are mixed, and the isomeric tridecanol polyoxyethylene ether TO-5 and the multi-branched isomeric tridecanol polyoxyethylene ether 1308 are added into the components TO interact, so that the molecules of the emulsifier can be rapidly diffused in the use process, the combination and aggregation of liquid drops are effectively prevented, the stability of the final emulsion is improved, and the stability of the low-temperature product can be further improved by adding the branched polyoxyethylene ether into the mixture.
The alkaline catalyst adopted by the self-made fatty alcohol polyvinyl ether provided by the invention ensures that the finally prepared fatty alcohol polyvinyl ether has narrow relative molecular mass distribution through the control of the temperature and the reaction time in the reaction process, and white oil, isomeric tridecanol polyoxyethylene ether TO-5 and multi-branched isomeric tridecanol polyoxyethylene ether 1308 are matched for use, so that the viscosity is moderate, and the fatty alcohol polyvinyl ether has better fluidity and stability at low temperature.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described below with reference to examples:
Example 1
The self-made fatty alcohol-polyoxyethylene ether is prepared by the following steps: the raw materials are the following raw materials in parts by weight
S1, sucking 180 parts of raw material C12-14 alcohol in an ethoxylation reaction device;
s2, adding 6 parts of an alkali metal catalyst KOH, dehydrating and circulating for more than 90 minutes at 120 ℃ by using a water ring vacuum pump, cooling to 80 ℃ and attempting to drop ethylene oxide, focusing on the temperature change of a reaction kettle heat exchanger at any time, controlling the temperature of a product in equipment to be 80+/-5 ℃, after 170 parts of ethylene oxide is dropped, preserving heat and curing, sampling and testing to be qualified, and cooling to 55 ℃ to obtain the fatty alcohol-polyoxyethylene ether. The time of heat preservation and curing in S2 is at least 30min.
The preparation method of the antifreeze type emulsifier for spinning sizing comprises the following steps:
The components in parts by weight are as follows
30 Parts of self-made fatty alcohol polyoxyethylene ether;
10 parts of isomeric tridecanol polyoxyethylene ether TO-5 isomeric alcohol ether;
8 parts of multi-branched chain isomerism tridecanol polyoxyethylene ether 1308;
10 parts of white oil;
Mixing to obtain the anti-freezing emulsifier for spinning sizing.
Example 2
The self-made fatty alcohol-polyoxyethylene ether is prepared by the following steps: the raw materials are the following raw materials in parts by weight
S1, sucking 180-220 parts of raw material C12-14 alcohol in an ethoxylation reaction device;
S2, adding 6 parts of alkali metal catalysts KOH and Ca (NO 3)2, at the temperature of 120 ℃, using a water ring vacuum pump to dehydrate and circulate for more than 90 minutes, cooling to the temperature of 80 ℃ to try to drop ethylene oxide, paying attention to the temperature change of a heat exchanger of a reaction kettle at the moment, controlling the temperature of products in equipment to be 80+/-5 ℃, after 170-210 parts of ethylene oxide is added, preserving heat and curing, sampling and testing to be qualified, and cooling to 55 ℃ to obtain the fatty alcohol polyoxyethylene ether, wherein the time of the heat preservation and curing in S2 is at least 30 minutes.
The preparation method of the antifreeze type emulsifier for spinning sizing comprises the following steps:
The components in parts by weight are as follows
32 Parts of self-made fatty alcohol polyoxyethylene ether;
12 parts of isomeric tridecanol polyoxyethylene ether TO-5 isomeric alcohol ether;
9 parts of multi-branched chain isomerism tridecanol polyoxyethylene ether 1308;
18 parts of white oil;
Mixing to obtain the anti-freezing emulsifier for spinning sizing.
Example 3
The self-made fatty alcohol-polyoxyethylene ether is prepared by the following steps: the raw materials are the following raw materials in parts by weight
S1, 220 parts of raw material C12-14 alcohol is sucked into an ethoxylation reaction device;
S2, adding 6-7.5 parts of alkali metal catalyst, namely KOH and Ca (NO 3)2, at the temperature of 120 ℃, using a water ring vacuum pump to dehydrate and circulate for more than 90 minutes, cooling to the temperature of 80 ℃ to try to drop ethylene oxide, paying attention to the temperature change of a heat exchanger of a reaction kettle at any time, controlling the temperature of a product in equipment to be 80+/-5 ℃, after 210 parts of ethylene oxide is added dropwise, preserving heat and curing, sampling and testing to be qualified, and cooling to 55 ℃ to obtain the fatty alcohol polyoxyethylene ether, wherein the time of preserving heat and curing is at least 30 minutes.
The preparation method of the antifreeze type emulsifier for spinning sizing comprises the following steps:
The components in parts by weight are as follows
40 Parts of self-made fatty alcohol polyoxyethylene ether;
15 parts of isomeric tridecanol polyoxyethylene ether TO-5 isomeric alcohol ether;
1308 10 parts of multi-branched-chain isomerism tridecanol polyoxyethylene ether;
20 parts of white oil;
Mixing to obtain the anti-freezing emulsifier for spinning sizing.
Comparative example 1
The self-made fatty alcohol-polyoxyethylene ether is prepared by the following steps: the raw materials are the following raw materials in parts by weight
S1, sucking 180-220 parts of raw material C12-14 alcohol in an ethoxylation reaction device;
S2, adding 6 parts of alkali metal catalysts KOH and Ca (NO 3)2, at the temperature of 120 ℃, using a water ring vacuum pump to dehydrate and circulate for more than 90 minutes, cooling to the temperature of 80 ℃ to try to drop ethylene oxide, paying attention to the temperature change of a heat exchanger of a reaction kettle at the moment, controlling the temperature of products in equipment to be 80+/-5 ℃, after 170-210 parts of ethylene oxide is added, preserving heat and curing, sampling and testing to be qualified, and cooling to 55 ℃ to obtain the fatty alcohol polyoxyethylene ether, wherein the time of the heat preservation and curing in S2 is at least 30 minutes.
The preparation method of the antifreeze type emulsifier for spinning sizing comprises the following steps:
The components in parts by weight are as follows
32 Parts of self-made fatty alcohol polyoxyethylene ether;
18 parts of white oil;
Mixing to obtain the anti-freezing emulsifier for spinning sizing.
Comparative example 2
The self-made fatty alcohol-polyoxyethylene ether is prepared by the following steps: the raw materials are the following raw materials in parts by weight
S1, sucking 180-220 parts of raw material C12-14 alcohol in an ethoxylation reaction device;
S2, adding 6 parts of alkali metal catalysts KOH and Ca (NO 3)2, at the temperature of 120 ℃, using a water ring vacuum pump to dehydrate and circulate for more than 90 minutes, cooling to the temperature of 80 ℃ to try to drop ethylene oxide, paying attention to the temperature change of a heat exchanger of a reaction kettle at the moment, controlling the temperature of products in equipment to be 80+/-5 ℃, after 170-210 parts of ethylene oxide is added, preserving heat and curing, sampling and testing to be qualified, and cooling to 55 ℃ to obtain the fatty alcohol polyoxyethylene ether, wherein the time of the heat preservation and curing in S2 is at least 30 minutes.
The preparation method of the antifreeze type emulsifier for spinning sizing comprises the following steps:
The components in parts by weight are as follows
32 Parts of self-made fatty alcohol polyoxyethylene ether;
9 parts of multi-branched chain isomerism tridecanol polyoxyethylene ether 1308;
18 parts of white oil;
Mixing to obtain the anti-freezing emulsifier for spinning sizing.
Comparative example 3
The self-made fatty alcohol-polyoxyethylene ether is prepared by the following steps: the raw materials are the following raw materials in parts by weight
S1, sucking 180-220 parts of raw material C12-14 alcohol in an ethoxylation reaction device;
S2, adding 6 parts of alkali metal catalysts KOH and Ca (NO 3)2, at the temperature of 120 ℃, using a water ring vacuum pump to dehydrate and circulate for more than 90 minutes, cooling to the temperature of 80 ℃ to try to drop ethylene oxide, paying attention to the temperature change of a heat exchanger of a reaction kettle at the moment, controlling the temperature of products in equipment to be 80+/-5 ℃, after 170-210 parts of ethylene oxide is added, preserving heat and curing, sampling and testing to be qualified, and cooling to 55 ℃ to obtain the fatty alcohol polyoxyethylene ether, wherein the time of the heat preservation and curing in S2 is at least 30 minutes.
The preparation method of the antifreeze type emulsifier for spinning sizing comprises the following steps:
The components in parts by weight are as follows
32 Parts of self-made fatty alcohol polyoxyethylene ether;
12 parts of isomeric tridecanol polyoxyethylene ether TO-5 isomeric alcohol ether;
18 parts of white oil;
Mixing to obtain the anti-freezing emulsifier for spinning sizing.
Comparative example 1 the formulation components in the comparative example are identical TO those of example 2 except that the emulsifier does not contain 130810 parts of isomeric trideceth polyoxyethylene ether TO-5 and of isomeric trideceth polyoxyethylene ether having multiple branches;
comparative example 2 the formulation components in the comparative example are identical TO those of example 2 except that the emulsifier does not contain isomeric trideceth TO-5 isomeric alcohol ether;
Comparative example 3 the formulation components of the comparative example were identical to those of example 2 except that the emulsifier did not contain the multi-branched isomeric tridecanol polyoxyethylene ether 1308;
6 centrifuge tubes were weighed, and 0.5g of deionized water was added to each of the sample tubes of the above examples and comparative examples. Placing the mixture in a constant-temperature water bath kettle at the temperature of 40-50 ℃, uniformly dispersing the solution by ultrasonic, recovering the solution to normal temperature, placing the mixture in an environment of-5 ℃ for 12 hours, and then placing the mixture at the normal temperature for checking.
Table 1 test results for examples 1 to 3 and comparative examples 1 to 2
The samples of examples 1 to 3 and comparative examples 1 to 3 were subjected to fiber spinning test on a tester, respectively, to observe the final properties. The products prepared by the treatment in the examples 1-3 have better flatness, smooth hand feeling and smooth post spinning. After the treatments of comparative examples 1 to 3, the yarn feel was unsmoothly produced during the preparation, and the yarn had a winding phenomenon during the spinning process, and the number of interruptions was large.
From the above table, the antifreeze type emulsifier for spinning sizing has the following advantages: the freezing-resistant emulsifier for spinning sizing is a nonionic emulsifier compounded by mixing fatty alcohol polyoxyethylene ether and white oil, and a product produced by low-temperature reaction has a more stable molecular structure, and ether bonds in the molecule are not easily damaged by acid and alkali, so that the emulsifier has the advantages of higher stability, good water solubility, electrolyte resistance, easiness in biodegradation and small foam, and simultaneously solves the problems that the traditional emulsifier is easy to generate layering and freezing in winter.
The self-made fatty alcohol polyvinyl ether and white oil are mixed, and the isomeric tridecanol polyoxyethylene ether TO-5 and the multi-branched isomeric tridecanol polyoxyethylene ether 1308 are added into the components TO interact, so that the molecules of the emulsifier can be rapidly diffused in the use process, the combination and aggregation of liquid drops are effectively prevented, the stability of the final emulsion is improved, and the stability of the low-temperature product can be further improved by adding the branched polyoxyethylene ether into the mixture.
The alkaline catalyst adopted by the self-made fatty alcohol polyvinyl ether provided by the invention ensures that the finally prepared fatty alcohol polyvinyl ether has narrow relative molecular mass distribution through the control of the temperature and the reaction time in the reaction process, and white oil, isomeric tridecanol polyoxyethylene ether TO-5 and multi-branched isomeric tridecanol polyoxyethylene ether 1308 are matched for use, so that the viscosity is moderate, and the fatty alcohol polyvinyl ether has better fluidity and stability at low temperature.
The emulsifier prepared by condensing natural fatty alcohol C12-14 alcohol serving as a synthesis initiator and ethylene oxide is a nonionic emulsifier, can be randomly prepared into an O/W type or W/O type emulsifier, can be randomly matched with other types of emulsifiers for use, and has extremely wide application range. The special emulsifier for spinning sizing, which is formed by compounding the produced fatty alcohol-polyoxyethylene ether with 10# white oil, isomeric tridecanol polyoxyethylene ether TO-5 isomeric alcohol ether and multi-branched isomeric tridecanol polyoxyethylene ether 1308, replaces the emulsifier made of sizing paste and animal and vegetable oil and the textile cream wax, and perfectly overcomes the defects that single yarn fibers are mutually cohesive and unstable, the surface hairiness is more and the spinning is difficult TO weave when spinning sizing is carried out. When the antifreeze emulsifier is applied to yarn slurry in winter, the emulsifier does not need to be baked in advance, a drying room does not need to be built, so that the labor and time are saved, the expenditure of the drying room can be saved, and multiple purposes are achieved. The non-ionic emulsifier has good acid and alkali resistance, is little influenced by salt and electrolyte, and has certain defoaming and antistatic effects, regardless of the pH value of the solution.
The foregoing description is only of the preferred embodiments of the present invention and is not intended to limit the scope of the invention, and all equivalent modifications made by the present invention are within the scope of the invention.

Claims (2)

1. The preparation method of the antifreeze type emulsifier for spinning sizing is characterized by comprising the following steps:
The components in parts by weight are as follows
30-40 Parts of self-made fatty alcohol polyoxyethylene ether;
10-15 parts of isomeric tridecanol polyoxyethylene ether TO-5;
8-10 parts of multi-branched-chain isomerism tridecanol polyoxyethylene ether 1308;
10-20 parts of white oil;
mixing to obtain the antifreeze type emulsifier for spinning sizing;
The self-made fatty alcohol-polyoxyethylene ether is prepared by the following steps:
The raw materials are the following raw materials in parts by weight
S1, sucking 180-220 parts of C12-14 alcohol serving as a raw material in an ethoxylation reaction device;
S2, adding 6-7.5 parts of alkali metal catalyst, dehydrating and circulating for more than 90 minutes at 120 ℃ by using a water ring vacuum pump, cooling to 80 ℃ and attempting to drop ethylene oxide, focusing on the temperature change of a reaction kettle heat exchanger at any time, controlling the temperature of a product in equipment to be 80+/-5 ℃, after 170-210 parts of ethylene oxide is dropped, preserving heat and curing, sampling and testing to be qualified, and cooling to 55 ℃ to obtain the fatty alcohol polyoxyethylene ether;
The alkali metal catalyst is KOH.
2. The method for preparing an emulsifier for sizing spun yarn according to claim 1, wherein the time of heat-preservation and aging in S2 is at least 30min.
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CN115305715A (en) * 2022-09-06 2022-11-08 安吉竹凯新材料科技有限公司 Water-soluble natural ester environment-friendly texturing oil and preparation method thereof

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CN111321599A (en) * 2020-04-10 2020-06-23 江门市润祥纺织科技有限公司 High-temperature-resistant alkali-resistant composite emulsifier for silicone oil emulsification and preparation method thereof
CN111996803A (en) * 2020-09-02 2020-11-27 多恩生物科技有限公司 Novel environment-friendly low-foam low-temperature degreasing agent and preparation method thereof
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GB725799A (en) * 1952-01-09 1955-03-09 Celanese Corp Textile lubricants
KR19990040635A (en) * 1997-11-19 1999-06-05 구광시 Emulsion composition for polyester fiber
CN103726327A (en) * 2013-10-10 2014-04-16 桐乡市恒隆化工有限公司 Environment-friendly composite type emulsifying agent
CN106750246A (en) * 2016-12-28 2017-05-31 桐乡市恒隆化工有限公司 A kind of frost resistance emulsifying agent and its production technology
CN107653671A (en) * 2017-08-03 2018-02-02 无锡嘉加科技有限公司 A kind of environment protection type multifunctional scouring agent and preparation method
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CN111996803A (en) * 2020-09-02 2020-11-27 多恩生物科技有限公司 Novel environment-friendly low-foam low-temperature degreasing agent and preparation method thereof
CN113789201A (en) * 2021-08-27 2021-12-14 成都科宏达化学有限责任公司 Antifreezing self-emulsifying white oil auxiliary agent and white oil solution

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