CN118029163A - High-temperature steaming-room-temperature stacking-physical scaling wool anti-felting finishing method based on broad-temperature-range protease - Google Patents
High-temperature steaming-room-temperature stacking-physical scaling wool anti-felting finishing method based on broad-temperature-range protease Download PDFInfo
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- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The invention relates to a high-temperature steaming-room-temperature stacking-physical scaling wool anti-felting finishing method based on broad-temperature protease, belonging to the field of dyeing and finishing of wool fabrics. The invention uses the reducer-protease composite working solution to pad the fabric, the working solution contains reducer, broad-temperature range protease, penetrating agent, strong protective agent and other components; after padding, a high-temperature steaming process is carried out, disulfide bonds and lipid structures in the wool scale layer are destroyed, and the hydrolysis efficiency of protease on the scale layer is improved; and (3) repeating the room temperature stacking procedure after padding the working solution, realizing full hydrolysis, stripping and falling of protease on wool scales under the limited field condition, and finally strengthening the anti-felting effect through the physical scaling process, so that the felting rate of the prepared wool fabric reaches the machine washable standard (felting rate is less than 6 percent), and the strength loss rate is lower (12 percent).
Description
Technical Field
The invention relates to a high-temperature steaming-room-temperature stacking-physical scaling wool anti-felting finishing method based on broad-temperature protease, belonging to the technical field of application of dyeing and finishing of wool fabrics in the wool spinning industry.
Background
In the textile industry, wool is a very important class of protein fibers with excellent drapability, warmth, acid resistance and moisture absorption properties. However, the wool fabric is washed to shrink and felt, so that the appearance changes such as shrinkage, wool surface hairiness and thickening, and blurred texture are caused, and the clothing performance of the fabric is seriously affected, so that the wool is required to be modified to improve the dimensional stability of the wool fabric.
At present, the modes for wool anti-felting finishing comprise three main types, namely 'subtraction' aiming at removing the wool scale layer, namely 'addition' of coating resin on the surface of the wool fabric, and 'addition and subtraction' of coating resin after removing the wool scale layer by combining the two methods. The most widely used industrial production is the chloridizing-Herbacea anti-felting technology, and the technology can effectively improve the dimensional stability of wool fabrics, but the wool fabrics treated by the technology are easy to absorb chlorine and yellow, have poor hand feeling and can generate absorbable organic halides (AOX) with great biological hazard.
As a non-chlorine shrink-proof process, the wool shrink-proof enzyme method has the advantages of mild action condition, high catalytic efficiency and environmental protection compared with the traditional chlorination process. The fabric subjected to shrink-proof finishing by an enzyme method has soft hand feeling and color luster. From the processing mode, the wool anti-felting enzyme method finishing can be classified into an impregnation method, a steaming method and a cold-stacking method. Compared with the dipping method, the steaming method and the cold-stacking method can obviously reduce the water consumption and sewage discharge in industrial production, reduce the circulating exchange of enzyme liquid and other reagents inside and outside the fabric, and reduce the hydrolysis to the inside of the fiber. However, the existing steaming process and cold pile process have a series of problems, which seriously affect the application and popularization of the process. The current steaming stacking process has strict requirements on temperature conditions, as patent CN 102965956A discloses a composite enzyme padding-steaming anti-felting process, and the steaming temperature is limited to 30-60 ℃; when the processing temperature exceeds 60 ℃, the anti-felting effect of the wool fabric can be seriously affected; in the wool fabric stacking process, a large amount of urea is often required to be used as a fiber swelling agent, and the concept of green and environment protection is not met.
There are many limitations to the wool anti-felting enzymatic finishing. From the point of action of the protease, the protease molecules, due to their small volume, are able to pass through the scaly layer, into the Cell Membrane Complex (CMC) and into the cortical layer inside the fiber. The leather layer has low sulfur content, is easily attacked by enzyme reagent, and causes hydrolysis and rupture of a large number of peptide bonds in the fiber, so that the wool fiber is severely and forcefully damaged; from the physical structure of wool, the wool flake layer comprises a flake surface layer, a flake outer layer and a flake inner layer, the flake surface layer contains 25% of lipoid structures, fatty acids such as 18-methyl eicosanoic acid (18-MEA) and the like which are main components of the wool can be subjected to thioester bond crosslinking with cystine residues of fibers, a layer of compact hydrophobic barrier is formed on the surfaces of the fibers, and the content of disulfide bonds and heterogeneous bonds in the flake outer layer is very high, so that the fibers have very strong resistance to water, chemical reagents and enzyme preparations due to the lipoid and disulfide bond structures.
Therefore, how to construct an enzyme method anti-felting method can limit protease on a flake layer on the surface of wool so as to reduce strength loss, and can increase the action sites of the enzyme on the wool flake layer so as to improve the stripping effect on wool flakes, which is a technical problem to be solved urgently.
Disclosure of Invention
Technical problems:
Aiming at the problems of large damage to the strong force of the existing enzymatic anti-felting finishing and low hydrolysis efficiency of scales, the invention provides the wool anti-felting finishing method, the felting rate of the prepared wool fabric is lower than 6%, the warp strong loss rate is lower than 12%, the alkali solubility is lower than 13.1%, and the machine washable standard can be achieved.
The technical scheme is as follows:
In one aspect, a wool anti-felting finishing process is provided, comprising the steps of:
(1) First padding of a reducing agent-protease composite working solution: soaking wool fabric in a reducing agent-protease composite working solution at 60-80 ℃ to fully wet the wool fabric, and carrying out twice soaking and twice rolling to obtain a liquid carrying rate of 70-80%; wherein the reducer-protease compound working solution comprises a reducer, broad-temperature-range protease, a penetrating agent and a strong protective agent; the broad-temperature-range protease can have more than 75% of relative enzyme activity at 25-80 ℃ and more than 90% of relative enzyme activity after heat preservation for 2 hours in the temperature range; the penetrating agent is polyoxyethylene nonionic surfactant with cloud point of 40-80 ℃;
(2) High temperature steaming: placing the wool fabric obtained in the step (1) in a steam environment at 60-90 ℃ for heat preservation for 20-120 min;
(3) The second padding reducing agent-protease composite working solution: repeating step (1);
(4) Stacking at room temperature: winding and piling the wool fabric obtained in the step (3) for 20-24 hours at room temperature;
(5) Physical scaling: and (3) carrying out acid washing and water washing on the wool fabric obtained in the step (4) to remove enzymolysis products and residual auxiliary agents on the wool fabric, and simultaneously, carrying out physical scaling through the mechanical friction effect between the cloth guide roller and the wool fabric.
In some embodiments, in the reductant-protease complex working fluid: the concentration of the reducing agent is 1-10 g/L; the enzyme activity of the broad temperature range protease is 10150U/mL, and the addition amount of the broad temperature range protease is 0.6-1.2 mL/L; the adding amount of the penetrating agent is 0.1-1 mL/L; the concentration of the strong protective agent is 0.5-2.5 g/L, and the pH value of the reducer-protease composite working solution is 8-9.
In some embodiments, the strong protectant is an anionic polymer having a molecular weight of 300-600 tens of thousands. For example, the strong protectant includes at least one of polyacrylic acid, polymethacrylic acid, polyvinylsulfonic acid, polystyrene sulfonic acid or anionic polyacrylamide having a molecular weight of 300 to 600 tens of thousands.
In some embodiments, the penetrating agent includes at least one of a polyoxyethylene ether of an alkylphenol, a fatty alcohol polyoxyethylene ether, a fatty acid methyl ester polyoxyethylene ether, or a fatty acid polyoxyethylene ether.
In some embodiments, step (1) and step (3) are performed in an open width padding unit, with a running cloth speed in the range of 50-60 m/min; step (2) is carried out in a steaming unit, and the running cloth speed range is 10-20 m/min; step (4) is carried out in a rotary stacking unit, and the rotation speed range is 20-40 rpm; the step (5) is carried out in a hexagonal roll type loose flat washer, and the running cloth speed range is 50-60 m/min.
In some embodiments, the step (5) specifically includes 3 washing steps, wherein washing liquid adopted in the 3 washing steps is pickling liquid, washing liquid a and washing liquid b in sequence, the time of each washing step is 10-15 min, and the temperature of the washing liquid is 30-35 ℃; simultaneously, the mechanical friction between the cloth guide roller and the wool fabric is utilized to physically strip scales; the step of physically peeling the scales is carried out in a hexagonal roll type loose flat washer, and the running cloth speed is 55m/min.
In some embodiments, the pickling solution comprises 0.05% to 0.1% acetic acid and 1% to 3% pancreatic bleach T; the washing liquid a contains 0.1-0.3 g/L Na 2CO3 and 1-3% of pancreatic bleaching T, and the washing liquid b contains 1-3% of pancreatic bleaching T; the pH of the pickling solution is 4-5, the pH of the washing solution a is 9-10, and the pH of the washing solution b is 6-7.
In some embodiments, the wool fabric comprises a worsted woolen fabric. For example, the wool fabric is full-wool thin tweed or full-wool medium-thickness tweed.
In another aspect, an anti-felting wool fabric produced by the foregoing process is provided.
The beneficial effects are that:
(1) Aiming at the problems of low hydrolysis efficiency and poor stripping effect of common protease on scales, the invention firstly screens the broad-temperature-range protease with high-temperature tolerance; the broad-temperature-range protease is a commercial enzyme detergent with higher tolerance to extreme environments, and the main component of the broad-temperature-range protease is serine endoprotease. The invention researches show that the broad-temperature-range protease has higher enzyme activity and temperature stability in a broad-temperature range of 25-80 ℃, and the retention rate of the enzyme activity is more than 90% after the broad-temperature-range protease is kept in a solution at 25-80 ℃ for 2 hours. The enzyme has poor temperature stability under the condition of 90 ℃ solution, and the retention rate of the enzyme activity is only 8.35% after 10min of heat preservation. The research of the invention also finds that the high-temperature steaming processing mode can improve the heat resistance of the broad-temperature-range protease, and the enzyme activity retention rate of the broad-temperature-range protease is 66.85% after the broad-temperature-range protease is kept in high-temperature steam at 90 ℃ for 1h, which is far higher than the enzyme activity retention rate in solution at 90 ℃, thus ensuring that the broad-temperature-range protease can play a role under the high-temperature steaming condition at 90 ℃. According to the invention, the high-temperature-resistant and reducing-agent-resistant broad-temperature-range protease is introduced into wool enzymatic anti-felting finishing for the first time, a high-temperature environment is provided by high-temperature steaming and stacking, the synergistic effect of a specific penetrating agent, a reducing agent and a strong protective agent is screened, the lipid structure of wool is destroyed, the accessibility of the broad-temperature-range protease to wool scales is increased, the action sites are increased, and the hydrolysis efficiency of the protease to the scales is improved;
(2) The invention uses the reducer-protease composite working solution to pad the fabric, the working solution contains reducer, broad-temperature range protease, penetrating agent, strong protective agent and other components; after padding, a high-temperature steaming process is carried out, disulfide bonds and lipid structures in the wool scale layer are destroyed, and the hydrolysis efficiency of protease on the scale layer is improved; the room temperature stacking procedure is carried out after the padding working solution is repeated, so that the wool flakes are fully hydrolyzed, peeled and shed by protease under the condition of limiting the domain; the invention weakens the trend of protease entering the cell membrane compound by selecting proper penetrating agent and strong protective agent, limits the effect of the protease to the wool flake layer, and reduces the damage to the internal structure of wool; the mechanical friction action of the hexagonal roller on the fabric is used for physically scaling, so that scaling which is in a tilted and loosened state is promoted, the anti-felting effect is enhanced, the obtained wool fabric product has excellent dimensional stability (felting rate is less than 6%), the warp strength loss rate is less than 12%, the alkali solubility is less than 13.1%, the strength is not obviously reduced, the machine washability standard can be still maintained at a higher level;
(3) Aiming at the problem that the strong damage is too large caused by the hydrolysis of the wool cell membrane compound and the leather layer by the protease in the traditional impregnation method, the invention uses the polyoxyethylene nonionic surfactant as the penetrating agent and the anionic polymer as the strong protective agent in combination, weakens the hydrolysis of the protease on the cell membrane compound in the fiber, and realizes the limited-domain hydrolysis of the wool scale layer within a wide temperature range; compared with the situation that the strength loss of the wool fabric product obtained by the traditional dipping method is larger (more than or equal to 20 percent), the value of the wool fabric product is obviously reduced (< 12 percent);
(4) The invention improves the defects of high-temperature steaming and room-temperature stacking, improves the optional range of steaming temperature, enables steaming to be carried out at a high temperature of 60-90 ℃, and reduces the dependence on swelling agent in the cold stacking process; meanwhile, the advantages of low water consumption and low sewage discharge are reserved, the utilization rate of protease is greatly improved, various requirements of open-width processing of wool fabrics in actual production can be met, and the method has high economic value;
(5) The protease belongs to a biocatalyst, has high catalytic efficiency, is ecological and environment-friendly, does not generate AOX in the reaction process, and accords with the concept of environmental protection better than the traditional chlorination method.
Detailed Description
Plain washing and boiling combination machine: the specific model is M flat washing and boiling combination machine, which consists of TECNOPLUS type flat washing machine and WPS type continuous woolen machine, and mainly comprises an open width padding unit, a steaming unit and a woolen boiling unit, wherein the fabric running speed of the open width padding unit is 0-80M/min, the fabric running speed of the steaming unit is 10-40M/min, the working width is 1200-2300 mm, and the equipment is purchased from Dalmedi (Beijing) mechanical equipment limited company.
Cold pad-batch dyeing machine: the specific model is CPB cold pad-batch dyeing machine, the main constituent units comprise an open width padding unit and a rotary stacking unit, the running cloth speed of the open width padding unit is 0-80 m/min, the working width is 1200-2300 mm, the rotating speed of the rotary stacking unit is 20-40 rpm, and the equipment is purchased from Union mechanical Co.
Hexagonal roller type loose flat washer: the specific model is S220-180 loose type open width cloth washer, which consists of a plurality of hexagonal roll type loose type open width washing tanks; the hexagonal roller overspeed is 7% -9% in the running process, the hexagonal roller has the functions of oscillating washing liquid and rubbing fabrics, the running cloth speed is 50-60 m/min, and the equipment is purchased from Jiangyin Fuda dyeing and finishing combined machinery Co.
Broad temperature range protease: the specific model isUno 100L is a commercial enzyme detergent, the main component of the commercial enzyme detergent is serine proteinase, the commercial enzyme detergent can be used in a wide temperature range of 20-80 ℃ and a wide pH range of 6-11, has good stability in reducing agents and chelating agents, the actual measured enzyme activity is 10150U/ml, and the enzyme preparation is purchased from NoveXin (China) investment Co.
The testing method comprises the following steps:
1. Felt shrinkage testing method
The dimensional stability of the washed fabric was determined with reference to GB 8628-2001 "preparation, marking and measurement of fabric samples and garments in test for dimensional Change of textiles" and GB 8629-2001 "household washing and drying procedure for textile test".
2. Breaking strength testing method
The breaking strength and the strength loss rate of the treated wool fabric are calculated by referring to GB/T6529-2008 Standard atmosphere for textile moisture control and test, GB/T3923.1-2013 determination of breaking strength and breaking elongation of the 1 st part of the tensile property of textile fabric (strip sample method).
3. Alkali solubility test method
The alkali solubility of the treated wool fabric was calculated with reference to GB/T7571-2008 "determination of solubility of wool in alkali".
Example 1
A high-temperature steaming-room temperature stacking-physical scaling wool anti-felting finishing method based on broad-temperature protease adopts a wool fabric raw material of full-wool thin tweed (197 g/m 2), and comprises the following steps:
(1) First padding of a reducing agent-protease composite working solution: soaking wool fabric in a reducing agent-protease compound working solution with the pH value of 9 at 80 ℃ for 30s, and carrying out twice soaking and twice padding, wherein the liquid carrying rate is 75%; the reducer-protease composite working solution comprises: 3g/L sodium sulfite (used as a reducing agent), 1.2mL/L broad temperature range protease with an enzyme activity of 10150U/mL, 1.8g/L anionic polyacrylamide with a molecular weight of 300 ten thousand (used as a strong protecting agent), 1mL/L Xin Guichun polyoxyethylene ether (JFC-6) (used as a penetrating agent); the first padding step of the reducing agent-protease composite working solution is carried out in an open width padding unit in an M flat washing and boiling combination machine, and the running cloth speed is 55M/min;
(2) High temperature steaming: placing the wool fabric obtained in the step (1) in a steam environment at 90 ℃ for heat preservation for 20min; the high-temperature steaming step is carried out in a steaming unit in the M flat washing and boiling combination machine, and the running cloth speed is 15M/min;
(3) The second padding reducing agent-protease composite working solution: the step (1) is repeated, the difference is that the wool fabric obtained in the step (2) is replaced, the step of padding the reducer-protease compound working solution for the second time is carried out in an open width padding unit in a CPB cold pad-batch dyeing machine, and the running cloth speed is 55m/min;
(4) Stacking at room temperature: winding and stacking the wool fabric obtained in the step (3), and placing the wool fabric in a room temperature (30 ℃) environment for stacking for 24 hours; the step of stacking at room temperature is carried out in a rotary stacking unit of a CPB cold pad-batch dyeing machine, and the rotation speed is 20rpm;
(5) Physical scaling: carrying out 3 washing procedures on the wool fabric obtained in the step (4), wherein washing liquid adopted in the 3 washing procedures is pickling liquid, washing liquid a and washing liquid b in sequence, the time of each washing procedure is 10min, and the temperature of the washing liquid is 30 ℃; simultaneously, physical scale stripping is carried out by utilizing the mechanical friction effect between the hexagonal cloth guide roller and the fabric, wherein the pickling solution contains 0.05% of acetic acid and 2% of pancreatic bleaching T; the washing liquid a contains 0.2g/L Na 2CO3 and 2% of pancreatic bleaching T, and the washing liquid b contains 2% of pancreatic bleaching T; the step of physically peeling the scales is carried out in a hexagonal roll type loose flat washer, and the running cloth speed is 55m/min.
Example 2
A broad-temperature-range protease-based high-temperature steaming-room-temperature stacking-physical scaling wool anti-felting finishing method is characterized in that the soaking temperature is adjusted to 60 ℃ in the steps of first padding reducing agent-protease compound working solution and second padding reducing agent-protease compound working solution, the steam temperature is adjusted to 60 ℃ in the high-temperature steaming step, and the steaming time is adjusted to 120min, and referring to example 1.
Example 3
A high-temperature steaming-room temperature stacking-physical scaling wool anti-felting finishing method based on broad-temperature protease adopts a wool fabric raw material of full-wool medium-thickness tweed (285 g/m 2), and comprises the following steps:
(1) First padding of a reducing agent-protease composite working solution: soaking wool fabric in a reducing agent-protease composite working solution with the pH value of 8 at 80 ℃ for 30s, and carrying out twice soaking and twice padding, wherein the liquid carrying rate is 75%; the reducer-protease composite working solution comprises: 7.25g/L L-cysteine hydrochloride, 1.2mL/L of broad-temperature-range protease with an enzyme activity of 10150U/mL, 1.5g/L of polymethacrylic acid with a molecular weight of 300 ten thousand, and 1mL/L of Xin Guichun polyoxyethylene ether (JFC-6) (used as a penetrating agent); the first padding step of the reducing agent-protease composite working solution is carried out in an open width padding unit in an M flat washing and boiling combination machine, and the running cloth speed is 55M/min;
(2) High temperature steaming: placing the wool fabric obtained in the step (1) in a steam environment at 90 ℃ for heat preservation for 20min; the high-temperature steaming step is carried out in a steaming unit in the M flat washing and boiling combination machine, and the running cloth speed is 15M/min;
(3) The second padding reducing agent-protease composite working solution: the step (1) is repeated, the difference is that the wool fabric obtained in the step (2) is replaced, the step of padding the reducer-protease compound working solution for the second time is carried out in an open width padding unit in a CPB cold pad-batch dyeing machine, and the running cloth speed is 55m/min;
(4) Stacking at room temperature: winding and stacking the wool fabric obtained in the step (3), and placing the wool fabric in a room temperature (30 ℃) environment for stacking for 24 hours; the step of stacking at room temperature is carried out in a rotary stacking unit of a CPB cold pad-batch dyeing machine, and the rotation speed is 20rpm;
(5) Physical scaling: carrying out 3 washing procedures on the wool fabric obtained in the step (4), wherein washing liquid adopted in the 3 washing procedures is pickling liquid, washing liquid a and washing liquid b in sequence, the time of each washing procedure is 10min, and the temperature of the washing liquid is 30 ℃; simultaneously, physical scale stripping is carried out by utilizing the mechanical friction effect between the hexagonal cloth guide roller and the fabric, wherein the pickling solution contains 0.05% of acetic acid and 2% of pancreatic bleaching T; the washing liquid a contains 0.2g/L Na 2CO3 and 2% of pancreatic bleaching T, and the washing liquid b contains 2% of pancreatic bleaching T; the step of physically peeling the scales is carried out in a hexagonal roll type loose flat washer, and the running cloth speed is 55m/min.
Comparative example 1
Comparative example 1 differs from example 1 in that the wool fabric was not subjected to any treatment.
Comparative example 2
A steaming-room temperature stacking-physical scaling wool anti-felting finishing method based on broad temperature range protease, referring to example 1, is different in that the soaking temperature is adjusted to 30 ℃ in the step of first padding reducing agent-protease compound working solution and the soaking temperature is adjusted to 30 ℃ in the step of steaming, and the steaming time is 120min.
Comparative example 3
A wool anti-felting finishing method is different from example 1 in that a soaking method is adopted to respectively perform pretreatment and enzyme treatment, and the specific process comprises the following steps:
(1) Dipping reducing agent working solution: immersing wool fabric in a reducing agent working solution with the temperature of 50 ℃ and the pH value of 11.3 for 1h to obtain a fabric pretreated by the reducing agent; wherein the reducing agent working fluid comprises: 10g/L sodium sulfite (used as reducing agent), 1mL/L Xin Guichun polyoxyethylene ether (JFC-6) (used as penetrating agent);
(2) And (3) cold water washing: fully washing the wool fabric obtained in the step (1) with cold water to remove redundant reducing agent;
(3) Impregnating protease working solution: immersing the wool fabric obtained in the step (2) in protease working solution with the pH value of 9 at the temperature of 80 ℃ for 30min; the protease working solution comprises broad temperature range protease with the concentration of 1.2mL/L and the enzyme activity of 10150U/mL, anionic polyacrylamide with the concentration of 1.8g/L and the molecular weight of 300 ten thousand (used as a strong protective agent), and Xin Guichun polyoxyethylene ether (JFC-6) with the concentration of 1mL/L (used as a penetrating agent);
(4) Physical scaling: carrying out 3 washing procedures on the wool fabric obtained in the step (3), wherein washing liquid adopted in the 3 washing procedures is pickling liquid, washing liquid a and washing liquid b in sequence, the time of each washing procedure is 10min, and the temperature of the washing liquid is 30 ℃; simultaneously, physical scale stripping is carried out by utilizing the mechanical friction effect between the hexagonal cloth guide roller and the fabric, wherein the pickling solution contains 0.05% of acetic acid and 2% of pancreatic bleaching T; the washing liquid a contains 0.2g/L Na2CO3 and 2% of pancreatic bleaching T, and the washing liquid b contains 2% of pancreatic bleaching T; the step of physically peeling the scales is carried out in a hexagonal roll type loose flat washer, and the running cloth speed is 55m/min.
Comparative example 4
A wool anti-felting finishing process differs from comparative example 4 in that the temperature of the impregnating protease working fluid is 90 ℃.
Comparative example 5
A wool anti-felting finishing method, comparative example 5 is different from example 1 in that (3) the steps of padding the reducing agent-protease composite working solution for the second time and (4) stacking at room temperature are omitted, and only steps (1), (2) and (5) are performed.
Comparative example 6
A wool anti-felting finishing method, comparative example 6 differs from example 1 in that (1) the steps of first padding the reducing agent-protease composite working solution and (2) high-temperature steaming are omitted, and only steps (3), (4) and (5) are passed.
Comparative example 7
A wool anti-felting finishing method is different from example 1 in that (1) the reducing agent-protease compound working solution for the first padding and (3) the reducing agent-protease compound working solution for the second padding are not added with any reducing agent.
Comparative example 8
A wool anti-felting finishing method is different from example 1 in that (1) the reducing agent-protease compound working solution for the first padding and (3) the reducing agent-protease compound working solution for the second padding are not added with any strong protective agent.
Comparative example 9
A wool anti-felting finishing method is different from example 1 in that (1) the reducing agent-protease compound working solution for the first padding and (3) the penetrating agent in the reducing agent-protease compound working solution used for the second padding are replaced by sodium dodecyl benzene sulfonate, and the concentration is 1g/L.
Comparative example 10
The wool anti-felting finishing method is characterized in that a reducing agent-enzyme mixing treatment is carried out by adopting an impregnation method in comparison example 10 and comparison example 3, and the specific process is as follows:
(1) The fabric was immersed in a reducing agent-protease complex working solution at 80 ℃ for 20min, the composition of the working solution being consistent with example 1.
(2) And (3) cold water washing: fully washing the wool fabric obtained in the step (1) with cold water to remove redundant reducing agent;
(3) Physical scaling: carrying out 3 washing procedures on the wool fabric obtained in the step (2), wherein washing liquid adopted in the 3 washing procedures is pickling liquid, washing liquid a and washing liquid b in sequence, the time of each washing procedure is 10min, and the temperature of the washing liquid is 30 ℃; simultaneously, physical scale stripping is carried out by utilizing the mechanical friction effect between the hexagonal cloth guide roller and the fabric, wherein the pickling solution contains 0.05% of acetic acid and 2% of pancreatic bleaching T; the washing liquid a contains 0.2g/L Na 2CO3 and 2% of pancreatic bleaching T, and the washing liquid b contains 2% of pancreatic bleaching T; the step of physically peeling the scales is carried out in a hexagonal roll type loose flat washer, and the running cloth speed is 55m/min.
The wool fabrics obtained in examples 1 to 3 and comparative examples 1 to 10 were subjected to measurement of felt rate, breaking strength loss rate and alkali solubility, and the results are shown in table 1.
TABLE 1 Performance test results
As can be seen from table 1:
a. The felting rate of the wool fabric samples (example 1, example 2 and example 3) prepared by the method is lower than 6%, the warp strength loss rate is lower than 12%, and the alkali solubility is lower than 13.1%, which proves that the wool fabric treated by the high-temperature steaming-room-temperature stacking-physical scaling process based on broad-temperature protease can reach the felting rate lower than 6%, the strength is not obviously reduced, the strength is still kept at a higher level, and the machine washable standard can be reached. Compared with the untreated wool fabric sample (comparative example 1), the felt rate was greatly reduced, which proves that the dimensional stability was greatly improved, and at the same time, the strength loss of the wool fabric was lower and the alkali solubility was not greatly changed.
B. Samples (comparative example 3, comparative example 4 and comparative example 10) treated by the traditional dipping process have the phenomena of higher felting rate (more than 6 percent) or higher strength loss rate (more than 15 percent) or higher two indexes, and the wool shrink-proof comprehensive performance is poor; this is probably due to the fact that in the dipping process, the fabric is contacted with a large amount of working fluid in the whole process, components such as reducing agent or enzyme in the working fluid can be circularly exchanged in the fabric, so that CMC in the fabric is severely damaged, and serious strong damage is easily caused to the fabric. The warp strength loss rates of comparative examples 3 and 10 were 20.20% and 25.00%, respectively; and the alkali solubility of comparative examples 3 and 10 was lower than that of untreated samples, mainly because: the wool fabric is severely damaged in structure during the impregnation process, and the wool fiber is partially dissolved during the treatment, so that the amount of soluble wool is reduced in the alkali solubility test.
C. The samples that were not subjected to the complete "high temperature steaming-room temperature stacking" treatment (comparative example 5, comparative example 6) had a reduced felting rate compared to the untreated samples (comparative example 1) but were still higher than 10%, demonstrating that the samples treated by either the high temperature steaming process (comparative example 5) or the room temperature stacking process (comparative example 6) alone failed to meet the "machine washable" standard, probably due to the following: the high-temperature steaming procedure can destroy part of lipoid and disulfide bonds, improve accessibility of protease to fabrics, and realize preliminary hydrolysis of wool scales; the room temperature stacking procedure can enable protease to be fully combined with sites on the scales, so that the wool scales are fully hydrolyzed under the condition of limiting the domain; it can be seen that both high temperature steaming and room temperature stacking are indispensable in the present invention.
D. The samples (comparative examples 7 and 8) which are not treated by the composite working solution containing complete components have the phenomena of higher felting rate (6%) or higher strength loss rate (15%), and can not reach the machine washable standard; the working solution in the comparative example 7 does not contain a reducing agent, so that disulfide bonds on the surface of wool cannot be reduced effectively, a wool scale layer still keeps a compact structure, and an enzyme reagent is difficult to act on the scale layer, so that the felting rate is higher (10.54 percent); the working fluid of comparative example 8 does not contain a strong protective agent, and the action of protease cannot be limited to the scale layer, so that the structures of the wool CMC and the inner leather layer are damaged, and the strong loss rate is higher (16.38%). Compared with a nonionic surfactant (Xin Guichun polyoxyethylene ether JFC-6), a sample (comparative example 9) treated by adopting an anionic surfactant (sodium dodecyl benzene sulfonate) is lower in strength loss, but the felting rate is 7.32%, and cannot reach the standard; the main reason may be that the broad temperature range protease used in the present invention has a lower stability in anionic surfactants than nonionic surfactants, and the anionic surfactants have a certain inhibition effect on the enzyme activity.
E. The present inventors have found that the broad temperature range protease used in the present invention has high temperature stability at 80℃and very poor temperature stability at 90℃based on the impregnation process, and that the 80℃treatment (comparative example 3) has a lower felting rate than 90℃in comparison with comparative example 4. The present study also found that the 90 ℃ treatment conditions (example 1) had lower felting rate and shorter action time compared to 60 ℃ (example 2) and 30 ℃ (comparative example 2) based on the high temperature steaming-room temperature stacking-physical descaling method. This is probably because the high-temperature steaming process can raise the heat resistance and the action temperature of the broad-temperature-range protease, so that the broad-temperature-range protease can act in a steam environment at 90 ℃, further breaking through the temperature limit in high-temperature steaming, and when the steam temperature is too low (for example, 30 ℃) (comparative example 2), lipid cannot be effectively dissolved, the reducing agent cannot effectively break disulfide bonds in the scale layer, and the degradation effect of the protease on the scale is greatly weakened. It follows that suitable steaming temperatures for the process according to the invention are 60 to 90 ℃.
The above examples are not intended to limit the scope of the invention nor the order of execution of the steps described. The present invention is obviously modified by a person skilled in the art in combination with the prior common general knowledge, and falls within the scope of protection defined by the claims of the present invention.
Claims (10)
1. A wool anti-felting finishing method is characterized by comprising the following steps:
(1) First padding of a reducing agent-protease composite working solution: soaking wool fabric in a reducing agent-protease composite working solution at 60-80 ℃ to fully wet the wool fabric, and carrying out twice soaking and twice rolling to obtain a liquid carrying rate of 70-80%; wherein the reducer-protease compound working solution comprises a reducer, broad-temperature-range protease, a penetrating agent and a strong protective agent; the broad-temperature-range protease can have more than 75% of relative enzyme activity at 25-80 ℃ and more than 90% of relative enzyme activity after heat preservation for 2 hours in the temperature range; the penetrating agent is polyoxyethylene nonionic surfactant with cloud point of 40-80 ℃;
(2) High temperature steaming: placing the wool fabric obtained in the step (1) in a steam environment at 60-90 ℃ for heat preservation for 20-120 min;
(3) The second padding reducing agent-protease composite working solution: repeating step (1);
(4) Stacking at room temperature: winding and piling the wool fabric obtained in the step (3) for 20-24 hours at room temperature;
(5) Physical scaling: and (3) carrying out acid washing and water washing on the wool fabric obtained in the step (4) to remove enzymolysis products and residual auxiliary agents on the wool fabric, and simultaneously, carrying out physical scaling through the mechanical friction effect between the cloth guide roller and the wool fabric.
2. The method according to claim 1, wherein in the reducing agent-protease complex working fluid: the concentration of the reducing agent is 1-10 g/L; the enzyme activity of the broad temperature range protease is 10150U/mL, and the addition amount of the broad temperature range protease is 0.6-1.2 mL/L; the adding amount of the penetrating agent is 0.1-1 mL/L; the concentration of the strong protective agent is 0.5-2.5 g/L, and the pH value of the reducer-protease composite working solution is 8-9.
3. The method of claim 1, wherein the strong protectant is an anionic polymer having a molecular weight of 300-600 tens of thousands.
4. The method of claim 3, wherein the strong protectant comprises at least one of polyacrylic acid, polymethacrylic acid, polyvinylsulfonic acid, polystyrene sulfonic acid, or anionic polyacrylamide having a molecular weight of 300-600 tens of thousands.
5. The method of claim 1, wherein the penetrating agent comprises at least one of a polyoxyethylene ether of an alkylphenol, a fatty alcohol polyoxyethylene ether, a fatty acid methyl ester polyoxyethylene ether, or a fatty acid polyoxyethylene ether.
6. The method according to claim 1, wherein the steps (1) and (3) are carried out in an open width padding unit, and the running cloth speed ranges from 50 to 60m/min; step (2) is carried out in a steaming unit, and the running cloth speed range is 10-20 m/min; step (4) is carried out in a rotary stacking unit, and the rotation speed range is 20-40 rpm; the step (5) is carried out in a hexagonal roll type loose flat washer, and the running cloth speed range is 50-60 m/min.
7. The method according to claim 1, wherein the step (5) comprises 3 washing steps, the washing liquid adopted in the 3 washing steps is pickling liquid, washing liquid a and washing liquid b in sequence, the time of each washing step is 10-15 min, and the temperature of the washing liquid is 30-35 ℃; simultaneously, the mechanical friction between the cloth guide roller and the wool fabric is utilized to physically strip scales; the step of physically peeling the scales is carried out in a hexagonal roll type loose flat washer, and the running cloth speed is 55m/min.
8. The method of claim 7, wherein the pickling solution comprises 0.05 to 0.1% acetic acid and 1 to 3% pancreatic bleaching T; the washing liquid a contains 0.1-0.3 g/L Na 2CO3 and 1-3% of pancreatic bleaching T, and the washing liquid b contains 1-3% of pancreatic bleaching T; the pH of the pickling solution is 4-5, the pH of the washing solution a is 9-10, and the pH of the washing solution b is 6-7.
9. The method of claim 1, wherein the wool fabric comprises a worsted woolen fabric.
10. An anti-felting wool fabric produced according to the process of any one of claims 1 to 9.
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