CN105887246B - A kind of cement products vinal spinning oil - Google Patents
A kind of cement products vinal spinning oil Download PDFInfo
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- CN105887246B CN105887246B CN201610271861.2A CN201610271861A CN105887246B CN 105887246 B CN105887246 B CN 105887246B CN 201610271861 A CN201610271861 A CN 201610271861A CN 105887246 B CN105887246 B CN 105887246B
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
- D01F11/04—Chemical after-treatment of artificial filaments or the like during manufacture of synthetic polymers
- D01F11/06—Chemical after-treatment of artificial filaments or the like during manufacture of synthetic polymers of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
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Abstract
The present invention relates to a kind of cement products vinal spinning oil, the finish is made up of spinning oil and post processing finish two parts, spinning oil is formed using macromolecule vegetable oil derivatives class surfactant and a small amount of fluorine-containing face activating agent, and post processing finish is made up of long chain fatty acyl amide cationic softener and antistatic additive.Less toxic, the low high-temperature volatile of spinning oil macromolecule surfactant, combined with the high osmosis of a small amount of fluorine surfactant, ensure that macromolecule finish spinnability and drawing by high temperature during low cigarette, low excitatory, reduce environmental pollution, improve working environment.The hydrophobicity of higher fatty acid amide and the oriented attachment of hydrophilic group cation parent's fiber in finish are post-processed, improves flatness, the antistatic behaviour of fiber, fibrous absorbent rate is reduced, improves the dispersiveness in cement；The shielding to fiber surface part of hydroxyl is provided simultaneously, reduces the interface binding force with coagulation soil matrix, increases cement products toughness.
Description
Technical field
The present invention relates to cement products technical field for building, especially a kind of cement products vinal spinning
Finish.
Background technology
Cement products polyvinyl alcohol (PVA) fiber is high strength high modulus PVA fiber, and manufacture method has six kinds：Wet method adds boron
Spinning, dry-wet spinning, gel spinning, phase separation spinning, crosslinking spinning, polyvinyl acetate alcoholysis direct spinning, at present I
State is based on use first method.
Wet method adds boron spinning to be to add boric acid in PVA solution as crosslinking agent, forms cross-linked gel structure with PVA, subtracts
Few macromolecular entanglements form highly oriented and highly crystalline high strength high modulus PVA fiber, typical process is as follows in favor of super drawing：
PVA powder → washing → dissolving → deaeration → spinning (alkaline coagulating bath) → damp and hot stretching → acid neutralization → damp and hot stretching
→ washing → oil → and oil → cut off → finished product for xeothermic stretching → xeothermic stretching (220~240 DEG C) →.
Whole technical process typically oils at twice, and oil needs finish to have good permeability for the first time, is tens thousand of
Fiber ectonexine can provide suitable smooth and coherent, eliminate electrostatic, to ensure not glue in dry and xeothermic drawing process
Even；Further, since 220~240 DEG C of drawing by high temperature, also requires that finish must have good heat resistance.Oil for the second time main
Antistatic behaviour, short fine laxity and the dispersiveness in cement during fibre cutting is provided.
At present, the document of research is less in terms of the domestic relevant finish delivered, and the main literature retrieved is as follows：
Patent No. ZL 201210079631.8, disclose a kind of vinal spinning oil for civil engineering
Agent, component composition：Antistatic additive-poly- cellulose quaternary ammonium salt, 16~30 parts；Emulsifying agent-mono- glycerine fatty acid (C8~C12)
Ester, 12~28 parts；Smooth agent-amino-modified silicone oil, 32~55 parts；Modifying agent-nano grade inorganic silica, 1~5 part.
Patent No. ZL 201210078776.6, disclose a kind of vinal for toughness reinforcing cement concrete and use
Spinning oil, component composition：Antistatic additive-fatty alkyl acyl hydramine, 16~30 parts；Smooth agent-C18~C22 ω -3 or ω -
6 unrighted acids, 12~28 parts；Stabilizer-alkyl polyoxyethylene ether, 32~55 parts；Additive-isobutyl group or n-octyl
Triethoxysilane, trifluoro propyl or trifluoro hexyl trimethoxy silane etc., 3~10 parts.
In two kinds of finishes, due to more (＞ 12%) containing the less composition of molecular weight, in 220 DEG C of xeothermic drawing processes
Middle smoke amount is larger.
In addition, two patents are respectively provided with surface modified function of the finish to fiber.Patent No. ZL201210079631.8
Composition containing " poly- cellulose quaternary ammonium salt " and " nano grade inorganic silica " polar group in disclosed finish, easily and cement
Hydrogen bond is formed between product and vinal surface great amount of hydroxy group after aquation, polyvinyl alcohol and cement is greatly improved
Cohesive force between concrete substrate.
The apolar substance that finish disclosed in patent No. ZL 201210078776.6 contains：Alkylalkoxy silane or halogen
Haloalkylalkoxysilane, the polar group on vinal surface can be played certain " screen effect ", avoid with
Basal body interface forms stress concentration, improves the toughness of cement concrete.
Effect of the fiber in cement matrix composite, is mainly manifested in：Toughness reinforcing, enhancing, resistance are split, and composite only has
The purpose that elongation strain hardening characteristics can be only achieved activeness and quietness can be produced.Fiber and the active force property at cement matrix interface
It may include：Friction cohesive force and few fibers when fiber and chemical adhesion, the fiber slippage at cement matrix interface are extracted
When sliding hardening.
Research shows, the hydroxyl of PVA fiber surfaces, can form hydrogen bond with the hydrated cement product in composite,
There is chemical binding layer between fiber and cement, tensile strength is set to be higher by hundred times, ten times of cement mortar respectively with modulus of elasticity
High-module high-strength PVA fibers, can effectively strengthen cement matrix composite.
But substantial amounts of hydroxyl is distributed with general undressed PVA fiber surfaces, makes a large amount of hydrated cement product accumulations
And tightly be bonded in fiber surface, fiber and cement concrete matrix is formed very strong chemical adhesion, cause stress
Concentrate, in tension, fiber is not drawn out easily, and majority is pulled off, and causes toughness reinforcing limited.
Early in 2001, existing foreign scholar was handled fiber surface with moderate lubrication oil, reduces fiber and water
The chemical adhesion of mud matrix, few fibers are made not to be pulled off when continuing development in crack, but from cement matrix
Extract, and there are stronger sliding hardening characteristics during extraction, thus make PVA composites in low fibers content
(2%) the single shaft limit tensile strain under the conditions of reaches 4%~8%.
In the case of finish disclosed in patent No. ZL 201210078776.6, smooth agent-docosahexaenoic acid, γ-
ω -3 or ω -6 unrighted acid of leukotrienes etc., additive-isobutyl group or n-octytriethoxysilane, trifluoro propyl
Or silane coupler such as trifluoro hexyl trimethoxy silane etc., the two combination, realize in spinning process to fiber surface hydroxyl
Shielding, reach toughness reinforcing purpose, it should be a kind of preferably selection, but two kinds of cost of material are higher, influence finish economy.
The content of the invention
The technical problem to be solved in the present invention is：Based on above mentioned problem, the present invention provides a kind of cement products polyethylene
Alcohol fibre spinning finish, high strength high modulus PVA fiber spinning is prepared for wet method plus boron spin processes, the present invention uses two kinds different groups
Into the finish of composition, meet fiber drawing process and fibre cutting and the requirement using process respectively, ensure the spinnability of fiber
With raising fiber performance, reduce environmental pollution, improve working environment.
The technical solution adopted for the present invention to solve the technical problems is：A kind of cement products vinal is provided
Spinning oil, high strength high modulus polyvinyl alcohol fiber spinning is prepared for wet method plus boron spin processes, spinning is completed using two kinds of finishes
Overall process, it forms as follows respectively：
Spinning oil：Consist of the following composition by weight percentage：
Polyglycereol double acid ester 40~50%；
The double APEOs 25~35% of pentaerythrite double acid ester；
Aliphatic acid polyethenoxy ether 15~25%；
Perfluoroalkyl ethanol APEO 0.05~0.15%；
Post-process finish：Double long-chains and single higher fatty acid amide base or fatty acid ester base class quaternary ammonium salt cationic surface-active
Agent composition, the two mixing ratio are 3：1~5：1.
Further, described polyglycereol double acid ester, pentaerythrite double acid ester double APEO, aliphatic acid
The stearic acid of aliphatic acid in APEO, specifically oleic acid, stearic acid or stearic acid content >=40% mixes with palmitic acid
One kind in acid；Glycerol polymerization degree in polyglycereol bis-fatty acid ester molecule is 4~6, pentaerythrite double acid ester double focusing oxygen
APEO mean molecule quantity is 600~800 in vinyl ether molecules, in the fatty acid molecule in aliphatic acid polyethenoxy ether
The average son amount of APEO is 1600~2500, the fluorine-containing carbon number of perfluoroalkyl in perfluoroalkyl ethanol APEO
For 6 or 8, APEO molecular weight is 200~400.
Described polyglycereol di fatty acid ester, glycerol polymerization degree are 4~6 polyglycereol oleic acid, stearic acid or stearic acid/palm fibre
The double acid ester of palmitic acid acid nitration mixture, there is provided good flatness；The double APEOs of described pentaerythrite double acid ester,
Polyethylene glycol total molecular weight per molecular is 1200~1600, there is provided good convergence；Described aliphatic acid polyoxy
Vinethene, the average son amount 1600~2500 of polyethers, there is provided good antistatic behaviour and coherent.
The design feature that fatty acid ester, nonionic, the molecular weight of three kinds of materials are big, polarity is larger, determines its tool
There is hypotoxicity, low volatility, low excitatory.
Hydrophobic group feedstock portions used in three kinds of surfactants are both from vegetable oil, and the first and second are the
Esterification process in prepared by one step only has water discharge environment, latter two basic three wastes during second step ethyleneoxide addition
Produce.Main material is renewable, production process low stain, the less harmful using process, belongs to green chemical.
Described perfluoroalkyl ethanol APEO, surface tension≤23dyn/cm of 0.001% concentration of aqueous solution, it is
Finish working solution provides good wetting, permeability.
Wet method adds in boron PVA spinning techniques oils position between washing and xeothermic stretching process first, in oil groove
The working solution that oils be the aqueous solution of active ingredient containing finish 0.8~1%.The tow of tens of thousands of fibers, it need to complete in seconds
Oil, it is desirable to which working solution there must be good wetting permeability, just can guarantee that the oil applying rate of fiber in tow table is basically identical.
If using conventional class wetting and penetrating agent instead, such as the less isomerous tridecanol polyoxyethylene of volatility (3~9) ether, if
Being maintained at 1% aqueous solution has compared with low surface tension, such as≤32dyn/cm, at least needs concentration of wetting agent >=0.1%, that is to say, that
At least need to account for the wetting and penetrating agent of the small-molecular-weight of finish total amount more than 10%.Such bleeding agent molecular weight is small, volatility is big,
It is also easy to produce more smog, excitatory big.
Molecules surfactant and 0.1% fluorocarbon surfactant group in this finish composition using more than 99%
Close, solve the contradiction of high volatile and rapid osmotic.
Further, described double higher fatty acid amide base or fatty acid ester base class quaternary cationicses are
Double fat acyloxy ethyls of double fatty acyl amido ethyl polyoxyethylene groups methylsulfuric acid ammonium methyls of logical formula (I), logical formula (II)
One kind in hydroxyethyl methyl sulfate methyl ammonium, double fat acyloxy ethyl alkyl dimethyl ammonium chlorides；
Fatty acyl amido RCONH in logical formula (I)-, or fatty acid-based RCOO in logical formula (II)-, it is from plant
One kind in C16~C18 saturated fatty acids of oil, n=3~6；
Described single higher fatty acid amide base or fatty acid ester base class quaternary cationics is stearmide
One kind in propyl-dimethyl-beta-hydroxyethyl ammonium dihydrogen orthophosphate, stearamidopropyl dimethyl-beta-hydroxyethyl ammonium nitrate.
Post-process double higher fatty acid amide base or fatty acid ester base class quaternary ammonium salt cationic surface-actives described in finish
Agent, it is the biodegradation type cationic softener that textile industry is used for textile soft finish, uses in this formula and also have
There are all characteristics of softening agent.The cationic and amido link of quaternary ammonium salt or the hydrogen bond Forming ability of ester bond, with having and viscose glue
The stronger negative electrical charge PVA fiber surfaces of the similar polyhydroxy of fiber, band, form the chemical binding force, hydrogen bond force and model moral of ionic bond
Hua Li, absorption fastness is big, is not easy to elute.The hydrophobicity of higher fatty acid amide and the oriented attachment of hydrophilic group cation parent's fiber,
Fiber surface tension force and coefficient of friction are reduced, water imbibition is reduced, improves antistatic behaviour.Fiber is set to be easier extended surface, increase
Its range of extension, increase flatness, reduce finished fiber and the phenomenon of uniting during silk and use, that is, add the short fibre of finished product
Laxity and the dispersiveness in cement.Because the softening agent with the oriented attachment of chemical bonds and is not easy to elute, shielding
The part of hydroxyl of fiber surface, the interface binding force with coagulation soil matrix is reduced, increase cement products toughness；
Polyoxyethylene groups polymerization degree n=3~6 in described softening agent, polyoxyethylene ether is introduced in the molecular structure, increase
Add its dispersiveness and Hydrophilic Fiber, wetability in water.N≤2, dispersiveness is bad in water；N >=7 influence absorption in fiber table
Washability behind face.
Post-process single higher fatty acid amide base or fatty acid ester base class quaternary ammonium salt cationic surface-active described in finish
Agent, it is the typical antistatic additive used in plastics or textile, such as：Stearamidopropyl dimethyl-beta-hydroxyethyl ammonium
Dihydrogen orthophosphate is antistatic additive SP, stearamidopropyl dimethyl-beta-hydroxyethyl ammonium nitrate is antistatic additive SN, with softness
Agent is used in combination, and increases its antistatic behaviour and wettability.
Antistatic additive SP and SN preparation process：Both first steps are identical, and with stearic acid and N, N- dimethylated propyl diethylenetriamines are
Raw material, carry out amidatioon generation SAPDMA；Second step, antistatic additive SP carry out quaternary ammonium with ethoxy phosphoric acid
Change and be made；Antistatic additive SN carries out quaterisation with oxirane and nitric acid and is made；The first step has esterification to generate water
Environment is discharged into, the basic three wastes of second step produce.
Above-mentioned soft, the cationoid surfactant of antistatic additive two, due to containing amido link or ester bond in molecular structure,
There is readily degradable.Raw material needed for synthesis is mainly the aliphatic acid for being derived from and being extracted in natural animal-plant oil, there is recyclability.Product
Plastics or rag trade use for many years, have security.So the raw material used in post processing finish is also for Green Chemistry
Product.
Because cationic surfactant mostly heat resistance is bad, using will break part-structure under the conditions of 200 DEG C of ＞
It is bad, so post processing finish is oiled after last xeothermic stretching together, before cut-out using spraying, reach drying using tow waste heat
Effect, and the stability of its finish structure can be kept.
Further, the average oil applying rate of described spinning oil is the 0.05%~0.25% of fiber dry weight, described
It is the 0.02%~0.1% of fiber dry weight to post-process the average oil applying rate of finish, and average always upper oil mass is 0.1%~0.3%.
The preceding spinning all nonionic surfactants of finish, there is good compatibility with post processing finish.
The beneficial effects of the invention are as follows：
1st, spinning oil is by macromolecular vegetable oil derivatives class non-ionic surface active and 0.1% organic fluoride class wetting agent
Combination, ensure that the spinnability of high-module high-strength PVA fibers, while there is low cigarette, low excitatory, reduce effect on environment；
2nd, finish is post-processed using degradable quaternary ammonium salt cationic softness/antistatic additive combination, and it is short to add PVA finished products
Fine dispersiveness and the toughness with cement composite material；
3rd, the raw material employed in finish is green chemical.
Embodiment
Presently in connection with specific embodiment, the invention will be further described, following examples be intended to illustrate invention rather than
Limitation of the invention further.
Embodiment 1
Spinning oil：
Formula：Double 16/18 nitration mixture ester 40kg of five polyglycereol, double polyoxyethylene (15) ethers of pentaerythritol dioleic acid ester
30kg, 16/18 nitration mixture polyoxyethylene (40) ether 30kg, perfluoro hexyl ethanol polyoxyethylene (5) ether 0.1kg.
Allotment：
Above-mentioned raw materials are sequentially added in stainless steel or enamel compounding kettle, are heated to 70 DEG C~75 DEG C, are melted to close to whole
Xie Hou, stirring is started, is stirred evenly, be cooled to less than 65 DEG C, discharging, filtering, packaging.
Quality index：
Outward appearance：Light yellow solid；Acid number：≤4mgKOH/g；Solid content：>=99.8%；
1% aqueous solution：
Outward appearance：Stable milky dispersion liquid；Viscosity：20~30mm2/s；Surface tension：≤32dyn/cm；PH value：7~
8。
Post-process finish：
Formula：It is stearic bicine diester amido ethyl polyoxyethylene groups (3) methylsulfuric acid ammonium methyl (content 90 ± 1%) 45kg, hard
Acyl amine propyl-dimethyl-beta-hydroxyethyl ammonium dihydrogen orthophosphate (content 40% ± 1) 25kg, water 30kg.It is (total：100kg)
Allotment：
Above-mentioned water and two kinds of materials are added into enamel or stainless steel compounding kettle, 50~60 DEG C is heated to, stirs evenly, discharging, mistake
Filter, packaging.
Quality index：
Outward appearance：Yellow emulsion；Solid content：50 ± 1%；Amine value：≤3mgKOH/g；PH value：5.5~7.
With the quality index of this finish spinning fibre：
Outward appearance：It is faint yellow；Fiber number：2.1dtex；Fracture strength：11.8cN/dtex；
Elongation at break：6.8%；Modulus：265cN/dtex；Hot water is reduced：1.8%；
Oil content：0.22%；Dispersiveness：1 grade；Shearing length：6mm.
Embodiment 2
Spinning oil：
Formula：The double stearates of five polyglycereol dioleic acid ester 48kg, pentaerythrite double polyoxyethylene (15) ether 22kg, tristearin
Sour polyoxyethylene (40) ether 30kg, perfluoro hexyl ethanol polyoxyethylene (5) ether 0.1kg.
Allotment：
Above-mentioned raw materials are sequentially added in stainless steel or enamel compounding kettle, are heated to 70 DEG C~75 DEG C, are melted to close to whole
Xie Hou, stirring is started, is stirred evenly, be cooled to less than 65 DEG C, discharging, filtering, packaging.
Quality index：
Outward appearance：Light yellow solid；Acid number：≤4mgKOH/g；Solid content：>=99.8%；
1% aqueous solution：
Outward appearance：Stable milky dispersion liquid；Viscosity：20~30mm2/s；Surface tension：≥32dyn/cm；PH value：7~
8。
Post-process finish：
Formula：Stearic bicine diester amido ethyl polyoxyethylene groups (6) methylsulfuric acid ammonium methyl (content 90 ± 1%) 55.6kg,
Stearamidopropyl dimethyl-beta-hydroxyethyl ammonium dihydrogen orthophosphate (content 40% ± 1) 25kg, water 39.4kg are (total：
120kg)。
Allotment：
Above-mentioned water and two kinds of materials are added into enamel or stainless steel compounding kettle, 50~60 DEG C is heated to, stirs evenly, discharging, mistake
Filter, packaging.
Quality index：
Outward appearance：Deep yellow emulsion；Solid content：50 ± 1%；Amine value：≤3mgKOH/g；PH value：5.5~7.
With the quality index of this finish spinning fibre：
Outward appearance：It is faint yellow；Fiber number：2.1dtex；Fracture strength：11.8cN/dtex；
Elongation at break：6.8%；Modulus：265cN/dtex；Hot water is reduced：1.8%；
Oil content：0.22%；Dispersiveness：1 grade；Shearing length：6mm.
By above-described embodiment 1 and embodiment 2, it can be seen that：The fiber spinned with this patent finish reaches textile industry mark
Alignment request (fiber check and measure method foundation：FZ/T 52023-2012 high-strength high-modulus polyethylene alcohol superbhort fiber).Dispersiveness reaches 1
Level, with present import finish effect it is suitable.
It is complete by above-mentioned description, relevant staff using the above-mentioned desirable embodiment according to the present invention as enlightenment
Various changes and amendments can be carried out without departing from the scope of the technological thought of the present invention' entirely.The technology of this invention
Property scope is not limited to the content on specification, it is necessary to determines its technical scope according to right.
Claims (3)
1. a kind of cement products vinal spinning oil, high-strength high-modulus polyethylene is prepared for wet method plus boron spin processes
Alcohol fibre spinning, it is characterised in that：Spinning overall process is completed using two kinds of finishes, it forms as follows respectively：
Spinning oil：Consist of the following composition by weight percentage：
Polyglycereol double acid ester 40~50%；
The double APEOs 25~35% of pentaerythrite double acid ester；
Aliphatic acid polyethenoxy ether 15~25%；
Perfluoroalkyl ethanol APEO 0.05~0.15%；
Post-process finish：Double long-chains mix with single higher fatty acid amide base or fatty acid ester base class quaternary cationics
Compound, the two mixing ratio are 3：1~5：1；
In described polyglycereol double acid ester, pentaerythrite double acid ester double APEO, aliphatic acid polyethenoxy ethers
Aliphatic acid, specifically one kind in the stearic acid of oleic acid, stearic acid or stearic acid content >=40% and palmitic acid mixed acid；It is poly-
Glycerol polymerization degree in glycerine bis-fatty acid ester molecule is 4~6, is gathered in pentaerythrite double acid ester double focusing oxygen vinyl ether molecules
Oxygen vinethene mean molecule quantity is 600~800, and the APEO in fatty acid molecule in aliphatic acid polyethenoxy ether is averaged
Son amount is 1600~2500, and the fluorine-containing carbon number of perfluoroalkyl in perfluoroalkyl ethanol APEO is 6 or 8, polyoxy second
Alkene ether molecular weight is 200~400.
A kind of 2. cement products vinal spinning oil according to claim 1, it is characterised in that：Described
Double higher fatty acid amide base or fatty acid ester base class quaternary cationicses are double fatty acyl amido second of logical formula (I)
Double fat acyloxy ethyl-hydroxyethyl methylsulfuric acid ammonium methyls, double of base polyoxyethylene groups methylsulfuric acid ammonium methyl, logical formula (II)
One kind in fat acyloxy ethyl alkyl dimethyl ammonium chloride；
Fatty acyl amido RCONH in logical formula (I)-, or fatty acid-based RCOO in logical formula (II)-, it is from vegetable oil
One kind in C16~C18 saturated fatty acids, n=3~6；
Described single higher fatty acid amide base or fatty acid ester base class quaternary cationics is stearamide propyl
One kind in dimethyl-beta-hydroxyethyl ammonium dihydrogen orthophosphate, stearamidopropyl dimethyl-beta-hydroxyethyl ammonium nitrate.
A kind of 3. cement products vinal spinning oil according to claim 1, it is characterised in that：Described
The average oil applying rate of spinning oil is the 0.05%~0.25% of fiber dry weight, and the average oil applying rate of described post processing finish is fibre
The 0.02%~0.1% of dry weight is tieed up, average always upper oil mass is 0.1%~0.3%.
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| US5973028A (en) * | 1997-06-13 | 1999-10-26 | Eastman Chemical Company | Yellow, hot melt adhesive traffic marking compositions |
| CN100378267C (en) * | 2006-07-14 | 2008-04-02 | 中国石油化工集团公司 | Oil agent used for polyester industrial filament |
| CN102720067B (en) * | 2012-03-22 | 2014-08-06 | 上海罗洋新材料科技有限公司 | Spinning oil for polyvinyl alcohol fiber in civil works |
| CN102936848B (en) * | 2012-11-19 | 2014-12-03 | 中国电建集团成都勘测设计研究院有限公司 | Method for modifying polyvinyl alcohol fibers and mass concrete with high crack resistance |
| CN103147168B (en) * | 2013-03-06 | 2017-06-16 | 常州市灵达化学品有限公司 | A kind of spinning oil and preparation method |
| CN103469571B (en) * | 2013-09-16 | 2015-10-14 | 天津工大纺织助剂有限公司 | A kind of water soluble vinylon finish and manufacture method thereof |
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