CN104611771A - Mulberry silk fiber oil removing and adhesive preserving process - Google Patents

Abstract

The invention provides a mulberry silk fiber oil removing and adhesive preserving process. The process is characterized by comprising the steps of presoaking, washing and dehydrating, softened water primary scouring, biological degenerating, washing and dehydrating, detergent washing, washing and dehydrating, cocoon cooking through a cocoon cooking machine, washing and dehydrating, softened water blanching, washing and dehydrating, softening, dehydrating and drying. By means of the process, the key technical problems of difficult decoloring, oil removing and adhesive preserving in scouring mulberry silkworm silk spinning raw materials in China are solved, the blank of processing the mulberry silkworm silk spinning raw materials at home is filled, more importantly, the problem of overstocking and sluggish sales of lots of silk spinning raw materials is solved, the utilization rate of mulberry silkworm defective cocoons, spun strips and frigons is increased, product quality and grade are improved, energy is saved, energy consumption is reduced, and the overall benefit of the sericulture is increased.

Description

Mulberry silk fiber deoils guarantor's adhesive process

Technical field

The present invention relates to mulberry silk fiber manufacture craft, be specifically related to a kind of mulberry silk fiber and deoil guarantor's adhesive process.

Background technology

Silk forms by wrapping up in silk gum outside 2 rhizoid elements, and silk gum weight accounts for 25%, fibroin weight accounts for 75%, and silk gum forms silk fiber outer tissue protein, is wrapped in around two rhizoid elements, plays a part protective effect and bonding silk fiber to fibroin.Silk gum has water-soluble, is soluble in hot water, acid, aqueous slkali, and fibroin can only part swelling and can not dissolving in water.On silk product, printing and dyeing practice for many years and the dress of dress ornament prove, content of silk gum is more than 5%, the gloss of silk can be affected, silk product easily decolours jaundice of hardening, and content of silk gum is lower than 3%, and silk fiber pulling force is inadequate, the crisp easy fracture of silk, have a strong impact on product service life.Silk fiber oil content is more than 0.5%, and spinnability is poor, easily causes entanglement, adhesion, hardens, drafting.Therefore telling silk spinning raw material spoiled cocoon, bar, in the refinery practice of basinetto silk, under the prerequisite removing grease (oil content controls below 0.5%), how could glue fat is retained within the scope of 3-5%, the difficult fat that removes photoresist of grease of silk fiber be difficult to ensure it is the technical barrier that silk spinning is produced always.

China is the cradle of Sericulture, is the maximum Silk quality producing country in the whole world and supply country, international Silk quality market is occupied leading status and absolute monopoly position, for major contribution has been made in national economy and foreign exchange earning.Because China silkworm produces new districtdevelopment rapidly, at present, production technology is delayed, production environment rather harsh, and working condition falls behind, and add the fluctuation of Cocoon Price, silk cocoon cocoon quality also exists the decline of different amplitude.In silk cocoon classification, silk cocoon is mainly divided into get on the bus cocoon and spoiled cocoon, and spoiled cocoon mainly comprises dupion, yellow spotted cocoon, cocoon pressed by cocooning frame, malformed cocoon, thin shelled cocoon, dead worm cocoon, maggot-pierced cocoon etc., along with the decline of cocoon quality, the ratio of spoiled cocoon constantly increases, and the thing followed is that knabs material also constantly increases.According to incompletely statistics, the annual silkworm spoiled cocoon produced in the whole nation is 5-6 ten thousand tons, and mulberry shoot is told, basinetto silk agreement that contracts a film or TV play to an actor or actress 50,000 tons.These large quantities of spoiled cocoons and mulberry shoot are told, basinetto silk sheet, can only carry out deep processing and become silk spinning raw material, be processed into Sang Mianqiu and cocoon silk quilt etc.On silk spinning raw material product, content of silk gum too much can affect the gloss of silk, and silk fiber easily hardens jaundice, and content of silk gum is very few, silk fiber pulling force not, easily crisp, have a strong impact on service life.Just because of silk spinning raw material kind is a lot, fibroin and content of silk gum are all not identical again, and refining process exists very big-difference.

Summary of the invention

Technical problem to be solved by this invention be how in processed filament fiber process not only except degrease but also reserve part silk gum, the functional characteristic of silk fiber is not fully exerted.

For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of mulberry silk fiber deoils guarantor's adhesive process, comprises following process:

Preimpregnation → flushing dehydration → demineralized water just white silk → biology corruption → rinse dehydration → washing → flushing dehydration → cocoon cooking machine cocoon cooking → flushing dehydration → demineralized water to bleach → rinse dehydration → softening → dehydration → oven dry, wherein:

Preimpregnation, at 6m ³general soaking pit in add sodium carbonate 2-4Kg, 105 washing agent 3-5kg, bar is told, basinetto silk, spoiled cocoon raw material at least one 100kg, and the liquid temperature in soaking pit is 50 DEG C-100 DEG C, preimpregnation time 12h, and pH value is 8;

Rinse dehydration, raw material dipped in advance is fully rinsed well de-dry;

Demineralized water is white silk just, is 3m at capacity ³conventional experienced bucket in add rinse dehydration after raw material 20 ㎏, add in bucket sodium carbonate 1 ㎏, 500 grams, 105 washing agent composition medicine auxiliary agent, bath raio reaches 1:100, and water temperature is 100 DEG C, and the time is 10min, and pH value is 10;

Biological corruption, capacity be 300 ㎏ degenerate in cylinders add demineralized water just practice after raw material 30 ㎏, add the auxiliary agent of sodium carbonate 400g, thunder rice side A 1kg composition again, molten ratio is 1:10, corruption time 72h, pH value is 9, cylinder temperature is 38 DEG C-40 DEG C, and insulation water temperature in cylinder periphery is 42 DEG C, turns over cylinder every day 2 times, heat 2 times, master cylinder peripheral temperature must not more than 42 DEG C;

Rinse dehydration, the raw material after being degenerated by biology is fully rinsed well de-dry;

Washing, the raw material of the eluting water that liquidates carries out washing, and washing water temperature is 65 DEG C, and the water yield is 3m ³, add hydrogen peroxide 2 ㎏ in water, sodium carbonate 500 grams, 105 500 grams, washing agent;

Rinse dehydration, the raw material after washing is fully rinsed well de-dry;

Cocoon cooking machine cocoon cooking, at capacity 2m ³cocoon cooking machine in add rinse dehydration after raw material 50 ㎏, then add sodium carbonate 1 ㎏, sulfur dioxide 100 grams, 500 grams, 105 washing agent composition medicine auxiliary agent, bath raio is 1:100, and water temperature is 100 DEG C, and the time is 30min, and pH value is 10;

Rinse dehydration, the raw material after cocoon cooking machine cocoon cooking is fully rinsed well de-dry;

Demineralized water is bleached, raw material after the eluting water that liquidates in Bellmer is bleached, according to Bellmer size constant volume, Bellmer remains 1/3 space, temperature is 85 DEG C, calculates with raw material weight proportioning, adds sodium carbonate 0.2%, hydrogen peroxide 25%, sodium silicate 10%, pancreas add the auxiliary agent that drift 0.3% forms; bath raio is 1:80, bleaching time 8h in Bellmer;

Rinse dehydration, the raw material after bleaching is fully rinsed well de-dry;

Softening, flood in softening cylinder, the water yield 300 ㎏ in cylinder, adding mulberry thin,tough silk soft dose of JS-203 is 400 grams, the glacial acetic acid 30-50 gram auxiliary agent formed, and bath raio is 1:10, and pH value is 4.5;

Dehydration, sloughs moisture content by the raw material after softening;

Dry, by the raw material stoving after dehydration, regain controls 10%.

The present invention is in silk spinning is produced, and concise object removes most of silk gum and grease, pigment, wax, inorganic matter and some other impurity on silk spinning raw material.According to the difference for the treatment of agent and method, can divide chemistry concise and concise two kinds of biology enzyme.Both containing basic group in the molecule of Bombyx-mori Silk Proteins, again containing acidic groups because of, therefore mulberry silk fiber is in different pH value solution, and can be combined with acid, can be combined with alkali again, this character is called the amphotericity of protein.Be in the protein in solution, neither with acid effect, again not with alkali effect, now the pH value of solution is called the isoelectric point of this protein.The isoelectric point of Bombyx mori Silk Fibroin is 2-3, and the isoelectric point of silk gum is 3.8-4.5.The pH value of concise liquid must away from isoelectric point, but in refinery practice, ph value is excessive or too smallly all can damage silk fiber.According to experimental study, pH value equal about 2 or 9.5-10.5 comparatively suitable.Due to the isoelectric point slant acidity of silk gum, it is stronger than acid is to the sensitiveness of alkali, so the multiplex alkali of refining process is practiced.

In refining process, coming unstuck deoils is two leading indicators, and silk gum is be wrapped in outside fibroin with gel state on silk, silk gum and fibroin all belong to protein, and fibroin is fibrous type protein, and chemical property is more stable, silk gum is ball-type protein, and chemical stability is poor.Coming unstuck is exactly the character utilizing silk gum soluble in water, by the effect of the chemical agents such as acid, alkali, impels it to dissolve, is hydrolyzed and reaches the object removed silk gum and retain fibroin.Some silk spinning raw material, because oozing out of pupal fat to stick on cocoon layer impact and produce and the quality of silk fiber, therefore must remove unnecessary pupal fat.Pupal fat is complicated higher fatty acids, the mixture of glyceride, under certain condition (catalytic action as water temperature, pressure or acid, alkali, enzyme) aliphatic acid and glycerine can be hydrolyzed into.Again because have usual auxiliaries sodium carbonate, washing agent, so the grease sticked on raw material just can be removed while coming unstuck under saponification and mechanism in the concise liquid come unstuck.

Mulberry silk fiber of the present invention deoils guarantor's adhesive process, thoroughly solve silk spinning raw material (tell containing spoiled cocoon, mulberry shoot, the mulberry basinetto silk) technical barrier that grease is high, glue fat is inadequate, oil content all controls less than 0.57%, gum content all more than 4.6%, fibre strength all reaches 3.7cN/dtex, average fiber length 78mm, cleannes are at 97 points, and various silk spinning raw material white silk folding all increases simultaneously.Technique of the present invention, not only solve in China's silkworm refining silk spinning raw material process decolour, the key technical problem of glue difficulty of deoiling, protect, fill up the blank of domestic processing silkworm silk spinning raw material, the more important thing is the difficult problem solving a large amount of silk spinning raw material overstocking and sluggish sale, improve silkworm spoiled cocoon, bar told, the utilization rate of basinetto silk, product quality and class are improved, and have saved the energy simultaneously, decrease energy consumption, improve the overall efficiency of silkworm industry.

Accompanying drawing explanation

Fig. 1 represents that mulberry silk fiber of the present invention deoils and protects the process chart of adhesive process.

Detailed description of the invention

Below in conjunction with accompanying drawing to mulberry silk fiber of the present invention deoil protect adhesive process illustrate.

Tradition mulberry silk fiber refining process is:

Corruption: often degenerate cylinder and to add water 300 ㎏, bath raio: 1:10, warm 38-40 DEG C in cylinder, peripheral temperature 42 DEG C

Auxiliary agent is sodium carbonate 500 grams;

Rinse de-dry: fully rinse dehydration well;

Washing: water temperature is 75 DEG C, every barrel adds sodium carbonate 1 ㎏, 105 washing agent 1 ㎏, corruption material 2 cylinder, time 30min, and pH value 10, works continuously;

Rinse de-dry: fully rinse dehydration well;

Cocoon cooking: water temperature 85 DEG C, bath raio 1:80, time 20min, auxiliary agent sodium carbonate 2 ㎏/bucket, 105 washing agent 1 ㎏, hydrosulfurous acid receives 50 grams/barrel;

Rinse de-dry: fully rinse dehydration well;

Bleaching: temperature 80-85 DEG C, bath raio 1:100, time 8h, auxiliary agent with raw material weight proportioning, sodium carbonate 0.2%, hydrogen peroxide 30%, sodium silicate 10%;

Rinse de-dry: fully rinse dehydration well;

Softening: the water yield 300 ㎏, molten than 1:10, pH value 4.5, JS-203 softener 400 grams, glacial acetic acid 30-50 gram;

Dewatered drying: slough moisture and dry, regain controls within 10%.

See Fig. 1, mulberry silk fiber of the present invention deoils guarantor's adhesive process, comprises following process:

Preimpregnation → flushing dehydration → demineralized water just white silk → biology corruption → rinse dehydration → washing → flushing dehydration → cocoon cooking machine cocoon cooking → flushing dehydration → demineralized water to bleach → rinse dehydration → softening → dehydration → oven dry.Wherein:

Preimpregnation, at 6m ³general soaking pit in add sodium carbonate 2-4Kg, 105 washing agent 3-5kg, bar is told, basinetto silk, spoiled cocoon raw material at least one 100kg, and the liquid temperature in soaking pit is 50 DEG C-100 DEG C, preimpregnation time 12h, and pH value is 8;

Rinse dehydration, raw material dipped in advance is fully rinsed well de-dry;

Demineralized water is white silk just, is 3m at capacity ³conventional experienced bucket in add rinse dehydration after raw material 20 ㎏, add in bucket sodium carbonate 1 ㎏, 500 grams, 105 washing agent composition medicine auxiliary agent, bath raio reaches 1:100, and water temperature is 100 DEG C, and the time is 10min, and pH value is 10;

Biological corruption, capacity be 300 ㎏ degenerate in cylinders add demineralized water just practice after raw material 30 ㎏, add the auxiliary agent of sodium carbonate 400g, thunder rice side A 1kg composition again, molten ratio is 1:10, corruption time 72h, pH value is 9, cylinder temperature is 38 DEG C-40 DEG C, and insulation water temperature in cylinder periphery is 42 DEG C, turns over cylinder every day 2 times, heat 2 times, master cylinder peripheral temperature must not more than 42 DEG C;

Rinse dehydration, the raw material after being degenerated by biology is fully rinsed well de-dry;

Washing, the raw material of the eluting water that liquidates carries out washing, and washing water temperature is 65 DEG C, and the water yield is 3m ³, add hydrogen peroxide 2 ㎏ in water, sodium carbonate 500 grams, 105 500 grams, washing agent;

Rinse dehydration, the raw material after washing is fully rinsed well de-dry;

Cocoon cooking machine cocoon cooking, at capacity 2m ³cocoon cooking machine in add rinse dehydration after raw material 50 ㎏, then add sodium carbonate 1 ㎏, sulfur dioxide 100 grams, 500 grams, 105 washing agent composition medicine auxiliary agent, bath raio is 1:100, and water temperature is 100 DEG C, and the time is 30min, and pH value is 10;

Rinse dehydration, the raw material after cocoon cooking machine cocoon cooking is fully rinsed well de-dry;

Demineralized water is bleached, raw material after the eluting water that liquidates in Bellmer is bleached, according to Bellmer size constant volume, Bellmer remains 1/3 space, temperature is 85 DEG C, calculates with raw material weight proportioning, adds sodium carbonate 0.2%, hydrogen peroxide 25%, sodium silicate 10%, pancreas add the auxiliary agent that drift 0.3% forms; bath raio is 1:80, bleaching time 8h in Bellmer;

Rinse dehydration, the raw material after bleaching is fully rinsed well de-dry;

Softening, flood in softening cylinder, the water yield 300 ㎏ in cylinder, adding mulberry thin,tough silk soft dose of JS-203 is 400 grams, the glacial acetic acid 30-50 gram auxiliary agent formed, and bath raio is 1:10, and pH value is 4.5;

Dehydration, sloughs moisture content by the raw material after softening;

Dry, by the raw material stoving after dehydration, regain controls 10%.

The present invention is told silkworm spoiled cocoon, mulberry shoot by above-mentioned process, mulberry is eliminated first-class silk fiber and samples respectively, tests, checks, and concrete inspection situation is as follows:

One, the mensuration of folding is practiced

1, the instrument and equipment used

(1), balance: scale division value≤0.01g;

(2), with the baking oven of balance.Balance: scale division value≤0.01g;

(3), container: capacity >=10L;

(4), heater: electric furnace;

(5), reagent: industrial neutral soap: fatty acids more than 60%, distilled water.

2, inspection procedure

(1), sample.The silkworm spoiled cocoon of different batches, mulberry shoot are told, mulberry eliminates first-class silk fiber and carry out sampling 500g ± 0.3g gram respectively, sample 50g ± 0.2g is got on the basis of the full-page proof obtained respectively, 10 samples got by each sample is one group, each sample divides two parts of samples, and every ten groups of assay weighted averages are result of the test.

(2), two parts of samples are put into constant temperature oven respectively, dry to constant weight by 120 ± 3 DEG C of temperature, be dry weight before practicing, then after according to the form below experimental condition puts into experienced liquid kiering twice respectively, fully wash with the distilled water of 65 ± 5 DEG C, again sample is placed in constant temperature oven, dries to constant weight by 120 ± 3 DEG C of temperature, be dry weight after practicing.Dry weight g × 100 before computing formula: residual silkgum content %=(before practicing, dry weight g-practices rear dry weight g) ÷ practices.Assay gets 2 significant digits.

With soap amount/(g/l)	Water quality	Bath raio	Temperature/DEG C	Time/min
					25	Distilled water	1：:200	98-100	30

3, assay is according to testing regulations, measure the residual silkgum content of different silk sample, through test of many times interpretation of result, measure silkworm spoiled cocoon residual silkgum content average out to 68.67%, the residual silkgum content average out to 21.11% that mulberry shoot is told, the residual silkgum content average out to 37.64% of mulberry basinetto silk sheet, reach a conclusion as silkworm spoiled cocoon, mulberry shoot is told, the experienced folding of mulberry basinetto silk is respectively 36.71%, 82.27%, 66.18%, and under traditional refining process, silkworm spoiled cocoon, mulberry shoot is told, the experienced folding of mulberry basinetto silk sheet is respectively 31.33%, 78.89%, about 62.36%, illustrate that silk fiber loses seriously in refinery practice, utilization rate is low.

Silkworm spoiled cocoon, mulberry shoot tell, mulberry basinetto silk practices folding detection case as table one.

Table one

Two, fracture strength inspection

1, instrument and equipment is used

(1), isodromicing elongation's test instrument (CRE): gauge length is 100mm, and the constant speed of dynamic folder support device movement is 150mm/min.Powerful accuracy of reading≤0.01kg(0.1N), elongation accuracy of reading≤0.1%;

(2), balance: scale division value≤0.01g;

(3), fiber number instrument scale division value≤0.5den;

(4), with the baking oven of balance.Balance: scale division value≤0.01g.

2, inspection procedure

(1), sampling, to different batches, different time, is told by silkworm spoiled cocoon, mulberry shoot, the concise every 10kg of the keen-witted and capable silk floss of mulberry silk processed of basinetto silk takes out a sample, each sample 250 grams ± 0.3g.

(2), weigh in the balance and count out sample gross weight after balance, sample carries out tension test one by one, test silk is divided equally, straight, make in order, put into upper and lower clamper, clamping degree of tightness is suitable, in jaw slippage and cut-out when preventing sample from stretching.Record maximum brute force and the most powerful time percentage elongation as the fracture strength of sample and elongation at break.

(3), fracture strength to get after decimal point 2.

Conventional process techniques silk fiber detection case is as table two.

Table two

Present invention process technology silk fiber detection case is as table three.

Table three

Three, cleannes inspection

1, the instrument and equipment used

(1), blackboard: long 1359mm, wide 463mm, thick 37mm(comprises frame), surface black is unglazed;

(2), control laboratory: the darkroom being provided with lighting fixture should completely cut off with extraneous light, and its wall, easel answer coating black lusterless paint, and uniform color is consistent.The easel left and right sides arranges screen, the upright each row of light echo lampshade, in-built daylight fluorescent lamp 3-4 or sky blue inside-frosted bulb 6, plate face average illumination is 400Lx, the illumination franchise ± 150Lx of blackboard upper and lower end and transverse axis center line, and blackboard left and right two ends illumination is basically identical.

2, inspection procedure

Inspection on cleanliness: inspector is positioned at distance blackboard 0.5m place, block-by-block inspection blackboard two sides, contrast cleanliness standard sample photograph, differentiates the type of clean fault, records its quantity respectively.Clean fault standard of deducting point: one point, each button of major defect, 0.4 point, each button of minor defect, 0.1 point, each button of common fault.Deduct the summation of all kinds of clean fault deduction of points with 100 points, be the clean achievement of this sample, point to represent, to get after decimal point 1.

Cleanliness factor is checked: select blackboard to live one side, vertical ground slopes inwardly about 5 DEG C, and inspector is positioned at distance blackboard 0.5m place, and according to the shape size of clean fault, quantity, distribution situation contrast neatness standard sample photograph, marks one by one.Best result is 100 points, is minimumly divided into 10 points, and more than 50 points, person every 5 is divided into 1 unit of marking, less than 50 points, every 10 are divided into 1 scoring unit.Calculate its mean value, be the isstudied of this sample.Point to represent, to get after decimal point 2, clean the cleannes achievement that achievement and isstudied two weighted averages are this sample.

In tradition refining process situation, the cleannes of different silkworm silk fiber are as table four.

Table four

The cleannes of present invention process different silkworm silk fiber are as table five.

Table five

Note: the weighted average being every 10 groups of samples above

Four, gum content inspection

1, the methods of sampling and quantity

Respectively from different batches, different time, told by silkworm spoiled cocoon, mulberry shoot respectively, keen-witted and capable continuous 10 full-page proofs of mulberry silk of mulberry basinetto silk sheet processing, each large sample is 500g ± 0.3g, then in each large sample, get sample 50g sample silk, be divided into two parts of samples, every part of sample 25g ± 0.2g.

2, the instrument and equipment used and reagent

(1), balance: scale division value≤0.01g;

(2), with the baking oven of balance.Balance scale division value≤0.01g;

(3), container: capacity >=10L;

(4), heater;

(5), timer;

(6), thermometer: scale division value is 1 DEG C.PH counts;

(9), reagent: Na ₂co _3,analyze pure, distilled water.

3, test method

(1), by 2 parts of samples mark respectively, be dried to dry weight, dry weight before claiming note to come unstuck;

(2), experiment condition: sodium carbonate 0.5g/L, water: distilled water, bath raio 1:100, temperature 98 ± 2 DEG C, time 30min;

(3), 2 parts have been claimed the sample of dry measure, by experimental condition, put into Na ₂come unstuck in CO3 solution, constantly stir with glass bar when coming unstuck, make to come unstuck evenly, fully wash with 50 DEG C of-60 DEG C of distilled water after coming unstuck.Come unstuck after secondary, clean, dry, weigh up dry measure after coming unstuck.

4, result of the test calculates

Dry measure × 100 before gum content=(dry measure before coming unstuck-come unstuck after dry measure) ÷ comes unstuck, result of calculation to be accurate to after decimal point 2.When two parts of sample gum contents differ by more than 3%, increase and take out the 3rd part of sample.

In conventional machining process situation, mulberry silk fiber gum content measures situation as table six.

Table six

Present invention process mulberry silk fiber gum content measures situation as table seven.

Table seven

Five, oil content inspection

1, the methods of sampling and quantity

Different time, different batches are told by silkworm spoiled cocoon, mulberry shoot, the keen-witted and capable silk floss of mulberry silk of mulberry basinetto silk sheet processing gets 10 full-page proofs, each full-page proof 500g ± 0.3g altogether, then in 10 full-page proofs, extract two samples respectively, each sample 50g ± 0.2g.

2, the instrument used, instrument and reagent

(1), soxhlet's extractor, accepting flask is 150 ml;

(2), analytical balance, scale division value is 0.1mg;

(3), thermostat water bath;

(4), constant temperature oven, temperature 105 DEG C ± 3 DEG C can be kept;

(5), drier, discolour silica gel is housed;

(6), vessel are weighed, qualitative filter paper;

(7) reagent: ether (chemical pure or analyze pure); Distilled water.

3, test method

(1), by accepting flask and weighing vessel be placed in the baking oven of 105 DEG C ± 3 DEG C and dry to constant weight, take quality and record;

(2), by each batch two parts of samples, wrap with qualitative filter paper, size, degree of tightness are suitable;

(3), on thermostat water bath soxhlet's extractor is installed, connects cooling water, heating water bath;

(4) dipping-sucking apparatus of soxhlet's extractor put into respectively by the sample two parts being surrounded by qualitative filter paper, then pours ether into, makes its submergence sample and exceed siphon pipe to produce backflow, connects condenser;

(5) regulate water bath heating temperature, make to accept the micro-Buddhist of ether in flask, keep backflow per hour 6 times-7 times, reflux 2h altogether;

(6), reflux complete, take off condenser, from dipping-sucking apparatus, take out sample, extract solvent, removing filter paper, puts into and weighs vessel, then connect condenser, reclaims ether;

(7), after ether volatilizees substantially, by being equipped with the weighing vessel of sample and accepting flask and be placed in the baking oven of 105 DEG C ± 3 DEG C and dry to constant weight, take out to weigh vessel and accept flask and puts into drier rapidly, be cooled to room temperature, take quality and record.Each sample constant weight beginning title time is about 120min, and during consecutive weighings, interval is about 25min;

(8), oil content calculates

The dry mass ÷ of the sample oil content=grease dry mass of sample (after the dry mass+degreasing of grease) × 100, calculate the arithmetic mean of instantaneous value of 2 parts of sample oil contents.

Indicate sample ID, numbering, weigh vessel, accept the quality of flask, the grease dry mass of every increment product, the dry mass of sample after glue fat, arithmetic mean of instantaneous value, reviewer and the date of inspection.

In tradition refining process situation, the oil content of mulberry silk fiber measures situation as table eight.

Table eight

The different mulberry silk fiber oil content of present invention process measures situation as table nine.

Table nine

The present invention increases raw material preimpregnation, demineralized water and just practices technique before traditional refining process biology corruption link.

Silk spinning raw material can be divided into three major types: spoiled cocoon, bar Tuhe basinetto silk, and spoiled cocoon is Shuan Gong, Chai Yin, oily rotten cocoon etc. mainly, and this kind of cocoon fat content is high, and silk fiber obtains severe contamination, can only have 30% for the silk fiber of silk spinning; Practice folding general about 40%; The byproduct of Tiao Tushi reeling mill, formed through manual tension by sleave out beating in silk reeling process, about the long general 1-1.5 rice of bar, two ends hang cocoon slightly individually, practice folding general about 80%, and basinetto silk is the left pelettes of reeling mill, form through basinetto silk mechanism sheet, upper with broken rotten silkworm chrysalis, glue fat is extremely heavy, practices folding one class about 50%.No matter what silk spinning raw material, production technology general is at present all directly boiling after biological corruption, directly white silk, unlike the height of kiering liquid temperature, the length of action time, chemical industry dosage use number different with the ratio of proportioning.

Corruption technique utilizes the metabolism of microorganism to generate enzyme, and sericin is hydrolyzed into soluble amino acid, while coming unstuck, is also broken down into aliphatic acid to grease, oil removing of coming unstuck completes simultaneously, and little to fibre damage.The internal and external temperature of general corruption cylinder is set in 38-40 DEG C and is conducive to microbial growth most, and when low temperature is long, corruption is come unstuck and deoiled very slowly, and usual bar is told, basinetto silk is degenerated and completed one-period in 48 hours, spoiled cocoon corruption needs 120 hours, for production, both consuming time long, waste energy again.Before biology corruption, increase preimpregnation just practice link, utilize the kiering waste liquid on the same day after the raw material preimpregnation will to produce for second day, just practicing, carry out biology corruption again, simultaneously with 5% thunder rice side A(soap class washing agent) as bleeding agent, so not only can shorten the time in corruption cycle 1/3rd, through appearance test and assay, the successful that deoils is better than traditional biological putrefaction.

The present invention improves the cocoon cooking of silk fiber, bleaching aqueous and cocoon cooking equipment, utilizes cocoon cooking machinery, demineralized water cocoon cooking and bleaching, solves silk fiber cleanliness factor and the inadequate problem of pulling force.

Tradition refining process is all directly boil straight drift, and the water quality of utilization is all underground water, and water quality is harder, and silk fiber is in improving technique situation, and preimpregnation and just white silk water are demineralized water, and possess uniform temperature, and the past all wastes.The present invention boils the requirement principle of drift to water quality according to silk fiber, determines to research and analyse boiling drift operation carries out.One is improve bleaching technology, and after biological corruption, pupal fat converts aliphatic acid to through decomposing, and part pupa skin and mummification material still remain in cocoon layer inside, is difficult to remove.In traditional bleaching technology, the bleaching agent mainly hydrogen peroxide (H that bleaching uses ₂o ₂), in silk bleaching process, hydrogen peroxide consumption generally adjusts between 20%-40%, but in actual tests, consumption, all about 80% time, just can reach obvious bleaching effect, cleanliness factor and whiteness reach requirement, but now silk fiber damage is excessive, and fiber strength obviously declines.Through lot of experiments and data analysis, in bleaching process, using Igepon T, (Igepon T i.e. 209 purification and washing agent, for anionic surfactant, be mainly used in the washing of wool, silk fabric, make it the sense with softness, gloss), it can improve the decomposing force of hydrogen peroxide, in the process of hydrogen peroxide bleaching, again impurity is emulsified in bleaching liquor, facilitates the decomposability of hydrogen peroxide.Two is change hard water directly to boil straight drift for demineralized water cocoon cooking bleaching; Three is independent research cocoon cooking machinery, reduces further silk fiber damage, adds cocoon cooking capacity, greatly reduce labour intensity.The present invention is by test of many times, and through the process modification of these two operations, institute practices the keen-witted and capable continuous quality of mulberry silk made and all can be up to state standards through checking indices, and the Sang Mianqiu quality of producing thus meets national standard.

Claims (1)

1. mulberry silk fiber deoils guarantor's adhesive process, it is characterized in that comprising following process:

Preimpregnation → flushing dehydration → demineralized water just white silk → biology corruption → rinse dehydration → washing → flushing dehydration → cocoon cooking machine cocoon cooking → flushing dehydration → demineralized water to bleach → rinse dehydration → softening → dehydration → oven dry, wherein:

Preimpregnation, at 6m ³general soaking pit in add sodium carbonate 2-4Kg, 105 washing agent 3-5kg, bar is told, basinetto silk, spoiled cocoon raw material at least one 100kg, and the liquid temperature in soaking pit is 50 DEG C-100 DEG C, preimpregnation time 12h, and pH value is 8;

Rinse dehydration, raw material dipped in advance is fully rinsed well de-dry;

Demineralized water is white silk just, is 3m at capacity ³conventional experienced bucket in add rinse dehydration after raw material 20 ㎏, add in bucket sodium carbonate 1 ㎏, 500 grams, 105 washing agent composition medicine auxiliary agent, bath raio reaches 1:100, and water temperature is 100 DEG C, and the time is 10min, and pH value is 10;

Biological corruption, capacity be 300 ㎏ degenerate in cylinders add demineralized water just practice after raw material 30 ㎏, add the auxiliary agent of sodium carbonate 400g, thunder rice side A 1kg composition again, molten ratio is 1:10, corruption time 72h, pH value is 9, cylinder temperature is 38 DEG C-40 DEG C, and insulation water temperature in cylinder periphery is 42 DEG C, turns over cylinder every day 2 times, heat 2 times, master cylinder peripheral temperature must not more than 42 DEG C;

Rinse dehydration, the raw material after being degenerated by biology is fully rinsed well de-dry;

Washing, the raw material of the eluting water that liquidates carries out washing, and washing water temperature is 65 DEG C, and the water yield is 3m ³, add hydrogen peroxide 2 ㎏ in water, sodium carbonate 500 grams, 105 500 grams, washing agent;

Rinse dehydration, the raw material after washing is fully rinsed well de-dry;

Cocoon cooking machine cocoon cooking, at capacity 2m ³cocoon cooking machine in add rinse dehydration after raw material 50 ㎏, then add sodium carbonate 1 ㎏, sulfur dioxide 100 grams, 500 grams, 105 washing agent composition medicine auxiliary agent, bath raio is 1:100, and water temperature is 100 DEG C, and the time is 30min, and pH value is 10;

Rinse dehydration, the raw material after cocoon cooking machine cocoon cooking is fully rinsed well de-dry;

Demineralized water is bleached, raw material after the eluting water that liquidates in Bellmer is bleached, according to Bellmer size constant volume, Bellmer remains 1/3 space, temperature is 85 DEG C, calculates with raw material weight proportioning, adds sodium carbonate 0.2%, hydrogen peroxide 25%, sodium silicate 10%, pancreas add the auxiliary agent that drift 0.3% forms; bath raio is 1:80, bleaching time 8h in Bellmer;

Rinse dehydration, the raw material after bleaching is fully rinsed well de-dry;

Softening, flood in softening cylinder, the water yield 300 ㎏ in cylinder, adding mulberry thin,tough silk soft dose of JS-203 is 400 grams, the glacial acetic acid 30-50 gram auxiliary agent formed, and bath raio is 1:10, and pH value is 4.5;

Dehydration, sloughs moisture content by the raw material after softening;

Dry, by the raw material stoving after dehydration, regain controls 10%.