CN109957861A - A kind of heat-resisting oxidation-resistance spinning oil - Google Patents
A kind of heat-resisting oxidation-resistance spinning oil Download PDFInfo
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- CN109957861A CN109957861A CN201910150358.5A CN201910150358A CN109957861A CN 109957861 A CN109957861 A CN 109957861A CN 201910150358 A CN201910150358 A CN 201910150358A CN 109957861 A CN109957861 A CN 109957861A
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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
- D01F11/08—Chemical after-treatment of artificial filaments or the like during manufacture of synthetic polymers of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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Abstract
The invention discloses a kind of heat-resisting oxidation-resistance spinning oils, belong to macromolecular fibre production technical field.The present invention activates Stropharia rugoso-annulata bacterium, fermented and cultured, it can produce a variety of organic matters, ketone and active matter such as laccase, during the ball milling material to grape pedicel carries out Microwave Extraction, more tannin can be leached, interaction between component, it is multi-level to improve to heat resistance and inoxidizability, with allyl-terminated polyether, containing hydrogen silicone oil etc. is raw material, it is blended by heat compound containing silicon material, pass through the accumulation of polyether segment and the reduction of nylon fibre contact angle, it is able to ascend its heat resistance, also the other components of this spinning oil can be improved for the function and effect of nylon fibre, various heat resistances and heat resistanceheat resistant performance for improving this spinning oil.Heat resistance, the inoxidizability that the present invention solves common spinning oil at present are poor, the problem of easily nylon fibre being made to turn yellow, caused damages.
Description
Technical field
The invention belongs to macromolecular fibre production technical fields, more particularly to a kind of heat-resisting oxidation-resistance spinning oil.
Background technique
Natural fiber passes through the basic material that the chemical fibre that extrusion obtains is textile industry.Strand and fiber add rear
Different mechanical force and thermal stress are subjected to during work.In order to ensure fiber is injury-free in this process, squeezed out in fiber
It should oil immediately after forming.Frictional property between the adjustable fiber of spinning oil and fiber, between fiber and metal, reduction rub
Coefficient is wiped, the electrostatic generated by friction is reduced, makes fiber that there is good convergence, flatness and fiber separation, after meeting fiber
Process relevant needs.As in reinforcing material such as nylon, artificial silk, in aramid fiber;Adhesive should be applied so that PET cord
It is adhered to rubber.In cord production, cord is enable to be adhered to water base Resorcin-Formaldehyde-Latex (RFL) gluing of rubber
Agent solution had been used more than 50 years.In RFL adhesive solvent, caustic alkali and ammoniac are most common catalyst.Institute
It states in solution, different formaldehyde/resorcinol (F/R) molar ratio, resin/latex ratio, solids ratios and other activity
Chemical substance is used in particular for PET fiber.Although the adherency of fiber such as nylon and artificial silk is easy to be adhered to rubber, PET with RFL
Fiber has any problem to the adherency of rubber.This main cause is and the functional group of RFL bonding such as carboxyl (COOH) and hydroxyl (OH)
Exist only in PET molecule chain end in PET fiber structure.In nylon and rayon material, the density of functional group is much higher than
In PET fiber.For this reason, the adhesive system of PET fiber is by Persisting exploitation.The method first is that exploitation spinning oil
Agent material will increase the surface-active of the RFL applied during PET fiber and yarn production.Spinning oil material is mostly
Liquid composition, it includes be more than a kind of ingredient and wherein all the components are in equilibrium state.Applying spinning oil material is
Very important part in fiber production process, provides fiber multiple performance, also by fiber surface and being present in life
Intermediate surface is formed between metal and/or ceramic composition during production to provide simply.The major function of spinning oil material is
By grease lubrication fiber surface to provide lubricating action, by reducing to the friction between Si-silk, silk-metal and silk-ceramics
Minimum provides fiber antistatic property with pre- anti-wear, and by keeping hundreds of silk to form fiber to prevent fiber from dissipating
Open (falling apart).Spinning oil has very important effect in high-performance fiber production, in spinning, stretches
With cause many problems in twisting process.These can be fibrous fracture, split silk, in tensile roller winding and roll form in
Uneven, twisting quality degradation and broken in (reel form) irregular, smoke, formation can not remove tar, roll form
It splits.For this reason, there should be some main performances for producing the spinning oil material of high quality fibers.Desired master
Wanting performance includes high decomposition temperature, high-incidence smoke temperature degree (smoking temperature), optimum viscosity, antistatic property etc..At present
Some conventional spinning oils in the market can occur seriously to smolder in use process, coking, lousiness, broken end, performance anti wicking are poor,
The problems such as polluting workshop condition.
Summary of the invention
The technical problems to be solved by the invention: it is poor for heat resistance, the inoxidizability of current common spinning oil, easily make
Nylon fibre turns yellow, and the problem of causing damages, provides a kind of heat-resisting oxidation-resistance spinning oil.
In order to solve the above technical problems, the present invention is using technical solution as described below:
A kind of heat-resisting oxidation-resistance spinning oil, according to the mass fraction, including following component: 2 ~ 5 parts of emulsifiers, 1 ~ 4 part of smooth agent,
3 ~ 7 parts of tert-butylhydroquinones, 0.2 ~ 0.5 part of sodium Diacetate, 1 ~ 4 part of dimethyl silicone polymer, 50 ~ 80 parts of deionized waters, also
Include: 25 ~ 40 parts of components of biomass, 18 ~ 30 parts it is compound containing silicon material.
The preparation method of the components of biomass, includes the following steps:
(1) it takes Stropharia rugoso-annulata bacterium powder 1:80 in mass ratio ~ 100 that water mixing is added, is seeded to activation culture by 2 ~ 4% inoculum concentration
Base obtains activation bacterium solution in 26 ~ 32 DEG C of activation cultures, takes activation bacterium solution to be seeded to fermentation medium by 2 ~ 4% inoculum concentration, in 28
~ 33 DEG C, shaken cultivation obtains fermentation liquid, takes fermentation liquid in 2 ~ 5 DEG C, centrifugal treating collects supernatant refrigeration, obtains active liquid;
(2) it takes grape pedicel 5 ~ 8:1 in mass ratio that ball-milling medium mixing is added, zirconia ball is added by ball 30 ~ 40:1 of material mass ratio
Pearl mixing is ground, ball milling obtains ball milling material, takes ball milling material 1:7 in mass ratio ~ 13 that acetone mixing, microwave treatment is added, and filtering takes filter
Active liquid, additive mixing is added in liquid 12 ~ 20:5:0.3 in mass ratio, adjusts pH, in 32 ~ 37 DEG C, oscillation treatment must be handled
Liquid is collected treatment fluid and is evaporated under reduced pressure to get components of biomass.
Activation medium in the step (1): according to the mass fraction, take 20 ~ 30 portions of potatos, 12 ~ 20 parts of glucose,
10 ~ 15 parts of peptones, 0.2 ~ 0.5 part of MgSO4, 0.1 ~ 0.4 part of KH2PO4, 600 ~ 800 parts of water mixing, sterilize to get activation culture
Base.
Fermentation medium in the step (1): according to the mass fraction, take 20 ~ 30 parts of cornstarch, 12 ~ 20 portions of sucrose,
10 ~ 15 parts of peptones, 0.2 ~ 0.5 part of casein, 0.1 ~ 0.4 part of KH2PO4, 600 ~ 800 parts of water mixing, sterilize to get activation culture
Base.
Ball-milling medium in the step (2): 6 ~ 10:1 in mass ratio takes ethanol solution, methylene chloride mixing to get ball
Grinding media.
Additive in the step (2): 1:2 ~ 5:0.2 in mass ratio takes triethanolamine, cetyl trimethyl bromination
Ammonium, lecithin mixing are to get additive.
Described compound containing silicon material preparation: 2 ~ 4:1 in mass ratio takes allyl-terminated polyether, containing hydrogen silicone oil mixing, in 50 ~ 70
DEG C, stirring is added the catalyst mixing of containing hydrogen silicone oil quality 3 ~ 7%, is warming up to 100 ~ 120 DEG C, and heat preservation obtains reaction material, negates and answer
Expect that beta-cyclodextrin is added in 15 ~ 25:1 in mass ratio ~ 4:1, lignin sulfonic acid is mixed and contains silicon material to get compound.
The catalyst: 1:15 ~ 25 take chloroplatinic acid, hexamethyldisilazane mixing to get catalyst in mass ratio.
The smooth agent: 2 ~ 5:1 in mass ratio takes olive oil, stearic amide mixing to get smooth agent.
The emulsifier: 3 ~ 7:2 in mass ratio takes laureth sodium sulfovinate, stearyl lactate mixing to get cream
Agent.
The present invention is compared with other methods, and advantageous effects are:
(1) present invention Stropharia rugoso-annulata bacterium is activated, fermented and cultured, can produce a variety of organic matters, ketone and active matter as paint
Enzyme can produce the function and effect that multiple action improves nylon fibre, carry out the process of Microwave Extraction in the ball milling material to grape pedicel
In, more tannin can be leached, has absorption to ultraviolet light, also, between tannin and tannin or tannin
Molecular complex can be formed with the effect of hydrophobic bond and hydrogen bond between fermentation gained letones, improve heat resistance, have
The presence of machine matter can also play coating function, and the protection of chemical bonding and physics aspect can be carried out to polyphenoils tannin,
Convenient for long-acting offer antioxidation, in addition, copigment chromatic effect altogether can occur for both one side tannin and letones each other,
It improves absorbance and improves its heat resistance, on the other hand also improve the workability inside this spinning oil, and make the two phase
Mutually collaboration, can stability and high efficiency improve the promotion of inoxidizability, heat resistance for nylon fibre, and a small amount of laccase is deposited
, it also may make part tannin that oxidation polymerization occurs, heat resistance can also be promoted by generating condensate, and to a certain degree
Under by heat effect, condensate can be analyzed to tannin etc. compared with small-molecule substance again, provide inoxidizability, avoid generating nylon fibre change
Huang, the problem of causing damages;
(2) present invention is blended compound containing silicon material, composition crosslinking work with allyl-terminated polyether, containing hydrogen silicone oil etc. for raw material by heat
With layer, its surface polar groups can be limited and migrated to the overturning of solid-air interface, its heat resistance is improved well, with this
Meanwhile by the accumulation of polyether segment and the reduction of nylon fibre contact angle, it is able to ascend its heat resistance, this spinning also can be improved
Function and effect of the other components of silk oil for nylon fibre, interaction, improvement of the raising to the heat-resisting oxidation-resistance of nylon fibre
Effect avoids the occurrence of nylon fibre flavescence, the problem of causing damages;
(3) present invention Stropharia rugoso-annulata bacterium is activated, fermented and cultured, and combine tannin, it is multi-level to improve to heat-resisting
Property and inoxidizability, make and compound it be able to ascend by the accumulation of polyether segment and the reduction of nylon fibre contact angle containing silicon material
Heat resistance, the other components of this spinning oil, which also can be improved, various can thus improve the function and effect of nylon fibre
The heat resistance and heat resistanceheat resistant performance of this spinning oil, avoiding the occurrence of common spinning oil at present easily makes brocade because heat resistance, inoxidizability are poor
Synthetic fibre yellowing of fibers, the problem of causing damages, improvement is significant.
Specific embodiment
Activation medium: according to the mass fraction, take 20 ~ 30 portions of potatos, 12 ~ 20 parts of glucose, 10 ~ 15 parts of peptones,
0.2 ~ 0.5 part of MgSO4, 0.1 ~ 0.4 part of KH2PO4, 600 ~ 800 parts of water mixing, in 121 DEG C of 12 ~ 20min of insulated sterilizing to get work
Change culture medium.
Fermentation medium: according to the mass fraction, take 20 ~ 30 parts of cornstarch, 12 ~ 20 portions of sucrose, 10 ~ 15 parts of peptones,
0.2 ~ 0.5 part of casein, 0.1 ~ 0.4 part of KH2PO4, 600 ~ 800 parts of water mixing, in 121 DEG C of 12 ~ 20min of insulated sterilizing to get activation
Culture medium.
Ball-milling medium: 6 ~ 10:1 in mass ratio takes the ethanol solution that volume fraction is 70%, methylene chloride to mix to get ball
Grinding media.
Additive: 1:2 ~ 5:0.2 in mass ratio takes triethanolamine, cetyl trimethylammonium bromide, lecithin mixing, i.e.,
Obtain additive.
Smooth agent: 2 ~ 5:1 in mass ratio takes olive oil, stearic amide mixing to get smooth agent.
Emulsifier: 3 ~ 7:2 in mass ratio takes laureth sodium sulfovinate, stearyl lactate mixing to get emulsifier.
Catalyst: 1:15 ~ 25 take chloroplatinic acid, hexamethyldisilazane mixing to get catalyst in mass ratio.
The preparation method of components of biomass, includes the following steps:
(1) it takes Stropharia rugoso-annulata bacterium powder 1:80 in mass ratio ~ 100 that sterile water mixing is added, is seeded to activation by 2 ~ 4% inoculum concentration
Culture medium, in 26 ~ 32 DEG C activation culture 3 ~ 5 days, obtain activation bacterium solution, take activation bacterium solution by 2 ~ 4% inoculum concentration be seeded to fermentation training
It supports base and, with 160 ~ 220r/min shaken cultivation 3 ~ 5 days, obtains fermentation liquid in 28 ~ 33 DEG C, take fermentation liquid in centrifuge, in 2 ~ 5 DEG C,
With 5000 ~ 8000r/min, 20 ~ 45min of centrifugal treating, supernatant is collected in 2 ~ 5 DEG C of refrigerator cold-storages, obtains active liquid;
(2) it takes grape pedicel 5 ~ 8:1 in mass ratio that ball-milling medium is added to mix in ball grinder, be added by ball 30 ~ 40:1 of material mass ratio
The mixing of zirconium oxide ball milling pearl, with 350 ~ 550r/min, 2 ~ 4h of ball milling, obtains ball milling material, and ball milling material 1:7 in mass ratio ~ 13 is taken to be added third
Ketone mixing moves to micro-wave oven with 400W 10 ~ 15min of microwave treatment, and filtering takes filtrate 12 ~ 20:5:0.3 to be in mass ratio added and lives
Property liquid, additive mixing, adjust pH to 6.3 ~ 6.7 with the citric acid solution that mass fraction is 20%, in 32 ~ 37 DEG C, with 180 ~
230r/min 40 ~ 60min of oscillation treatment, obtains treatment fluid, collect treatment fluid be evaporated under reduced pressure in 30 ~ 45 DEG C to the 25 of original volume ~
40% to get components of biomass.
Compound to prepare containing silicon material: 2 ~ 4:1 in mass ratio takes allyl-terminated polyether, containing hydrogen silicone oil to mix in reaction kettle, in 50 ~
70 DEG C, with 500 ~ 800r/min, 15 ~ 25min of magnetic agitation, the catalyst mixing of containing hydrogen silicone oil quality 3 ~ 7% is added, is warming up to
100 ~ 120 DEG C, 20 ~ 45min is kept the temperature, reaction material is obtained, takes reaction material 15 ~ 25:1 in mass ratio ~ 4:1 that beta-cyclodextrin, wooden is added
Plain sulfonic acid mixing contains silicon material with 2000 ~ 3000r/min magnetic agitation, 30 ~ 55min to get compound.
A kind of heat-resisting oxidation-resistance spinning oil, according to the mass fraction, including following component: 2 ~ 5 parts of emulsifiers, 1 ~ 4 part it is flat
Lubrication prescription, 3 ~ 7 parts of tert-butylhydroquinones, 0.2 ~ 0.5 part of sodium Diacetate, 1 ~ 4 part of dimethyl silicone polymer, 50 ~ 80 parts of deionizations
Water, 25 ~ 40 parts of components of biomass, 18 ~ 30 parts it is compound contain silicon material.
Embodiment 1
Activation medium: according to the mass fraction, 20 portions of potatos, 12 parts of glucose, 10 parts of peptones, 0.2 part of MgSO are taken4、0.1
Part KH2PO4, 600 parts of water mixing, in 121 DEG C of insulated sterilizing 12min to get activation medium.
Fermentation medium: according to the mass fraction, take 20 parts of cornstarch, 12 portions of sucrose, 10 parts of peptones, 0.2 part of casein,
0.1 part of KH2PO4, 600 parts of water mixing, in 121 DEG C of insulated sterilizing 12min to get activation medium.
Ball-milling medium: 6:1 in mass ratio takes the ethanol solution that volume fraction is 70%, methylene chloride mixing to get ball milling Jie
Matter.
Additive: 1:2:0.2 in mass ratio take triethanolamine, cetyl trimethylammonium bromide, lecithin mixing to get
Additive.
Smooth agent: 2:1 in mass ratio takes olive oil, stearic amide mixing to get smooth agent.
Emulsifier: 3:2 in mass ratio takes laureth sodium sulfovinate, stearyl lactate mixing to get emulsifier.
Catalyst: 1:15 in mass ratio takes chloroplatinic acid, hexamethyldisilazane mixing to get catalyst.
The preparation method of components of biomass, includes the following steps:
(1) it takes Stropharia rugoso-annulata bacterium powder 1:80 in mass ratio that sterile water mixing is added, is seeded to activation medium by 2% inoculum concentration,
In 26 DEG C activation culture 3 days, obtain activation bacterium solution, activation bacterium solution taken by 2% inoculum concentration to be seeded to fermentation medium, in 28 DEG C, with
160r/min shaken cultivation 3 days, fermentation liquid is obtained, takes fermentation liquid in centrifuge, in 2 DEG C, with 5000r/min centrifugal treating 20min,
Supernatant is collected in 2 DEG C of refrigerator cold-storages, obtains active liquid;
(2) it takes grape pedicel 5:1 in mass ratio that ball-milling medium is added to mix in ball grinder, zirconium oxide is added by ball material mass ratio 30:1
The mixing of ball milling pearl, with 350r/min ball milling 2h, obtains ball milling material, takes ball milling material 1:7 in mass ratio that acetone mixing is added, moves to microwave
Furnace is taken filtrate 12:5:0.3 in mass ratio that active liquid, additive mixing is added, is used quality with 400W microwave treatment 10min, filtering
The citric acid solution that score is 20% adjusts pH to 6.3 and, with 180r/min oscillation treatment 40min, obtains treatment fluid in 32 DEG C, collects
Treatment fluid is evaporated under reduced pressure to original volume in 30 DEG C 25% to get components of biomass.
Compound to prepare containing silicon material: 2:1 in mass ratio takes allyl-terminated polyether, containing hydrogen silicone oil to mix in reaction kettle, in 50 DEG C,
With 500r/min magnetic agitation 15min, the catalyst mixing of containing hydrogen silicone oil quality 3% is added, is warming up to 100 DEG C, keeps the temperature 20min,
Reaction material is obtained, takes reaction material 15:1:1 in mass ratio that beta-cyclodextrin, lignin sulfonic acid mixing is added, is stirred with 2000r/min magnetic force
30min is mixed to get compound containing silicon material.
A kind of heat-resisting oxidation-resistance spinning oil, according to the mass fraction, including following component: 2 parts of emulsifiers, 1 part of smooth agent,
3 parts of tert-butylhydroquinones, 0.2 part of sodium Diacetate, 1 part of dimethyl silicone polymer, 50 parts of deionized waters, 25 parts of biomass at
Point, 18 parts it is compound contain silicon material.
Embodiment 2
Activation medium: according to the mass fraction, 30 portions of potatos, 20 parts of glucose, 15 parts of peptones, 0.5 part of MgSO are taken4、0.4
Part KH2PO4, 800 parts of water mixing, in 121 DEG C of insulated sterilizing 20min to get activation medium.
Fermentation medium: according to the mass fraction, take 30 parts of cornstarch, 20 portions of sucrose, 15 parts of peptones, 0.5 part of casein,
0.4 part of KH2PO4, 800 parts of water mixing, in 121 DEG C of insulated sterilizing 20min to get activation medium.
Ball-milling medium: 10:1 in mass ratio takes the ethanol solution that volume fraction is 70%, methylene chloride to mix to get ball milling
Medium.
Additive: 1:5:0.2 in mass ratio take triethanolamine, cetyl trimethylammonium bromide, lecithin mixing to get
Additive.
Smooth agent: 5:1 in mass ratio takes olive oil, stearic amide mixing to get smooth agent.
Emulsifier: 7:2 in mass ratio takes laureth sodium sulfovinate, stearyl lactate mixing to get emulsifier.
Catalyst: 1:25 in mass ratio takes chloroplatinic acid, hexamethyldisilazane mixing to get catalyst.
The preparation method of components of biomass, includes the following steps:
(1) it takes Stropharia rugoso-annulata bacterium powder 1:100 in mass ratio that sterile water mixing is added, is seeded to activation culture by 4% inoculum concentration
Base, in 32 DEG C activation culture 5 days, obtain activation bacterium solution, take activation bacterium solution by 4% inoculum concentration to be seeded to fermentation medium, in 33
DEG C, with 220r/min shaken cultivation 5 days, fermentation liquid is obtained, takes fermentation liquid in centrifuge, in 5 DEG C, with 8000r/min centrifugal treating
45min collects supernatant in 5 DEG C of refrigerator cold-storages, obtains active liquid;
(2) it takes grape pedicel 8:1 in mass ratio that ball-milling medium is added to mix in ball grinder, zirconium oxide is added by ball material mass ratio 40:1
The mixing of ball milling pearl, with 550r/min ball milling 4h, obtains ball milling material, takes ball milling material 1:13 in mass ratio that acetone mixing is added, moves to micro-
Wave furnace is taken filtrate 20:5:0.3 in mass ratio that active liquid, additive mixing is added, is used matter with 400W microwave treatment 15min, filtering
The citric acid solution that amount score is 20% adjusts pH to 6.7 and, with 230r/min oscillation treatment 60min, obtains treatment fluid in 37 DEG C, receives
Collect treatment fluid in the 40% of 45 DEG C of reduction vaporization to original volume to get components of biomass.
Compound to prepare containing silicon material: 4:1 in mass ratio takes allyl-terminated polyether, containing hydrogen silicone oil to mix in reaction kettle, in 70 DEG C,
With 800r/min magnetic agitation 25min, the catalyst mixing of containing hydrogen silicone oil quality 7% is added, is warming up to 120 DEG C, keeps the temperature 45min,
Reaction material is obtained, takes reaction material 25:4:1 in mass ratio that beta-cyclodextrin, lignin sulfonic acid mixing is added, is stirred with 3000r/min magnetic force
55min is mixed to get compound containing silicon material.
A kind of heat-resisting oxidation-resistance spinning oil, according to the mass fraction, including following component: 5 parts of emulsifiers, 4 parts of smooth agents,
7 parts of tert-butylhydroquinones, 0.5 part of sodium Diacetate, 4 parts of dimethyl silicone polymers, 80 parts of deionized waters, 40 parts of biomass at
Point, 30 parts it is compound contain silicon material.
Embodiment 3
Activation medium: according to the mass fraction, 25 portions of potatos, 15 parts of glucose, 13 parts of peptones, 0.3 part of MgSO are taken4、0.2
Part KH2PO4, 700 parts of water mixing, in 121 DEG C of insulated sterilizing 16min to get activation medium.
Fermentation medium: according to the mass fraction, take 25 parts of cornstarch, 15 portions of sucrose, 13 parts of peptones, 0.3 part of casein,
0.2 part of KH2PO4, 700 parts of water mixing, in 121 DEG C of insulated sterilizing 15min to get activation medium.
Ball-milling medium: 8:1 in mass ratio takes the ethanol solution that volume fraction is 70%, methylene chloride mixing to get ball milling Jie
Matter.
Additive: 1:3:0.2 in mass ratio take triethanolamine, cetyl trimethylammonium bromide, lecithin mixing to get
Additive.
Smooth agent: 3:1 in mass ratio takes olive oil, stearic amide mixing to get smooth agent.
Emulsifier: 4:2 in mass ratio takes laureth sodium sulfovinate, stearyl lactate mixing to get emulsifier.
Catalyst: 1:17 in mass ratio takes chloroplatinic acid, hexamethyldisilazane mixing to get catalyst.
The preparation method of components of biomass, includes the following steps:
(1) it takes Stropharia rugoso-annulata bacterium powder 1:90 in mass ratio that sterile water mixing is added, is seeded to activation medium by 3% inoculum concentration,
In 28 DEG C activation culture 4 days, obtain activation bacterium solution, activation bacterium solution taken by 3% inoculum concentration to be seeded to fermentation medium, in 29 DEG C, with
180r/min shaken cultivation 4 days, fermentation liquid is obtained, takes fermentation liquid in centrifuge, in 3 DEG C, with 6000r/min centrifugal treating 35min,
Supernatant is collected in 3 DEG C of refrigerator cold-storages, obtains active liquid;
(2) it takes grape pedicel 6:1 in mass ratio that ball-milling medium is added to mix in ball grinder, zirconium oxide is added by ball material mass ratio 35:1
The mixing of ball milling pearl, with 450r/min ball milling 3h, obtains ball milling material, takes ball milling material 1:9 in mass ratio that acetone mixing is added, moves to microwave
Furnace is taken filtrate 16:5:0.3 in mass ratio that active liquid, additive mixing is added, is used quality with 400W microwave treatment 13min, filtering
The citric acid solution that score is 20% adjusts pH to 6.5 and, with 190r/min oscillation treatment 50min, obtains treatment fluid in 35 DEG C, collects
Treatment fluid is evaporated under reduced pressure to original volume in 35 DEG C 30% to get components of biomass.
Compound to prepare containing silicon material: 3:1 in mass ratio takes allyl-terminated polyether, containing hydrogen silicone oil to mix in reaction kettle, in 6 DEG C,
With 700r/min magnetic agitation 20min, the catalyst mixing of containing hydrogen silicone oil quality 5% is added, is warming up to 110 DEG C, keeps the temperature 35min,
Reaction material is obtained, takes reaction material 19:2:1 in mass ratio that beta-cyclodextrin, lignin sulfonic acid mixing is added, is stirred with 2500r/min magnetic force
45min is mixed to get compound containing silicon material.
A kind of heat-resisting oxidation-resistance spinning oil, according to the mass fraction, including following component: 3 parts of emulsifiers, 2 parts of smooth agents,
5 parts of tert-butylhydroquinones, 0.3 part of sodium Diacetate, 3 parts of dimethyl silicone polymers, 60 parts of deionized waters, 30 parts of biomass at
Point, 20 parts it is compound contain silicon material.
Comparative example 1: it is essentially identical with the preparation method of embodiment 1, it has only the difference is that lacking components of biomass.
Comparative example 2: it is essentially identical with the preparation method of embodiment 1, it has only the difference is that lacking compound containing silicon material.
Comparative example 3: the spinning oil of Shanghai City company production.
The spinning oil that above-described embodiment is obtained with comparative example is detected, test technology: spinning speed 3500m/
Min, 285 DEG C of spinning temperature plus bullet speed 550m/min, compare examination with the spinning oil that embodiment and comparative example obtain
It tests.As a result such as the following table 1.
Table 1:
In summary, spinning oil effect of the invention is more preferable as can be seen from Table 1, is worth of widely use, the foregoing is merely
Preferred mode of the invention, is not intended to limit the invention, all within the spirits and principles of the present invention, made any to repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of heat-resisting oxidation-resistance spinning oil, according to the mass fraction, including following component: 2 ~ 5 parts of emulsifiers, 1 ~ 4 part it is smooth
Agent, 3 ~ 7 parts of tert-butylhydroquinones, 0.2 ~ 0.5 part of sodium Diacetate, 1 ~ 4 part of dimethyl silicone polymer, 50 ~ 80 parts of deionized waters,
It is characterized by further comprising: 25 ~ 40 parts of components of biomass, 18 ~ 30 parts it is compound contain silicon material.
2. a kind of heat-resisting oxidation-resistance spinning oil according to claim 1, which is characterized in that the preparation of the components of biomass
Method includes the following steps:
(1) it takes Stropharia rugoso-annulata bacterium powder 1:80 in mass ratio ~ 100 that water mixing is added, is seeded to activation culture by 2 ~ 4% inoculum concentration
Base obtains activation bacterium solution in 26 ~ 32 DEG C of activation cultures, takes activation bacterium solution to be seeded to fermentation medium by 2 ~ 4% inoculum concentration, in 28
~ 33 DEG C, shaken cultivation obtains fermentation liquid, takes fermentation liquid in 2 ~ 5 DEG C, centrifugal treating collects supernatant refrigeration, obtains active liquid;
(2) it takes grape pedicel 5 ~ 8:1 in mass ratio that ball-milling medium mixing is added, zirconia ball is added by ball 30 ~ 40:1 of material mass ratio
Pearl mixing is ground, ball milling obtains ball milling material, takes ball milling material 1:7 in mass ratio ~ 13 that acetone mixing, microwave treatment is added, and filtering takes filter
Active liquid, additive mixing is added in liquid 12 ~ 20:5:0.3 in mass ratio, adjusts pH, in 32 ~ 37 DEG C, oscillation treatment must be handled
Liquid is collected treatment fluid and is evaporated under reduced pressure to get components of biomass.
3. a kind of heat-resisting oxidation-resistance spinning oil according to claim 2, which is characterized in that the activation in the step (1)
Culture medium: according to the mass fraction, 20 ~ 30 portions of potatos, 12 ~ 20 parts of glucose, 10 ~ 15 parts of peptones, 0.2 ~ 0.5 part are taken
MgSO4, 0.1 ~ 0.4 part of KH2PO4, 600 ~ 800 parts of water mixing, sterilize to get activation medium.
4. a kind of heat-resisting oxidation-resistance spinning oil according to claim 2, which is characterized in that the fermentation in the step (1)
Culture medium: according to the mass fraction, 20 ~ 30 parts of cornstarch, 12 ~ 20 portions of sucrose, 10 ~ 15 parts of peptones, 0.2 ~ 0.5 portion of junket are taken
Element, 0.1 ~ 0.4 part of KH2PO4, 600 ~ 800 parts of water mixing, sterilize to get activation medium.
5. a kind of heat-resisting oxidation-resistance spinning oil according to claim 2, which is characterized in that the ball milling in the step (2)
Medium: 6 ~ 10:1 in mass ratio takes ethanol solution, methylene chloride mixing to get ball-milling medium.
6. a kind of heat-resisting oxidation-resistance spinning oil according to claim 2, which is characterized in that the addition in the step (2)
Agent: 1:2 ~ 5:0.2 in mass ratio takes triethanolamine, cetyl trimethylammonium bromide, lecithin mixing to get additive.
7. a kind of heat-resisting oxidation-resistance spinning oil according to claim 1, which is characterized in that described compound containing silicon material preparation:
2 ~ 4:1 in mass ratio takes allyl-terminated polyether, containing hydrogen silicone oil mixing, and in 50 ~ 70 DEG C, containing hydrogen silicone oil quality 3 ~ 7% is added in stirring
Catalyst mixing, be warming up to 100 ~ 120 DEG C, heat preservation obtains reaction material, takes reaction material 15 ~ 25:1 in mass ratio ~ 4:1 that β-is added
Cyclodextrin, lignin sulfonic acid, which are mixed, contains silicon material to get compound.
8. a kind of heat-resisting oxidation-resistance spinning oil according to claim 7, which is characterized in that the catalyst: in mass ratio
1:15 ~ 25 take chloroplatinic acid, hexamethyldisilazane mixing to get catalyst.
9. a kind of heat-resisting oxidation-resistance spinning oil according to claim 1, which is characterized in that the smooth agent: in mass ratio 2
~ 5:1 takes olive oil, stearic amide mixing to get smooth agent.
10. a kind of heat-resisting oxidation-resistance spinning oil according to claim 1, which is characterized in that the emulsifier: in mass ratio
3 ~ 7:2 takes laureth sodium sulfovinate, stearyl lactate mixing to get emulsifier.
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