CN115897265A - Anionic hand feeling finishing agent and preparation method thereof - Google Patents
Anionic hand feeling finishing agent and preparation method thereof Download PDFInfo
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- CN115897265A CN115897265A CN202211691628.1A CN202211691628A CN115897265A CN 115897265 A CN115897265 A CN 115897265A CN 202211691628 A CN202211691628 A CN 202211691628A CN 115897265 A CN115897265 A CN 115897265A
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Abstract
The invention discloses an anionic hand feeling finishing agent and a preparation method thereof, wherein the anionic hand feeling finishing agent comprises an additive shown as a structural formula I:
wherein R =
Description
Technical Field
The invention relates to the technical field of textile after-finishing, in particular to an anionic hand feeling finishing agent and a preparation method thereof.
Background
The better softening finishing processing of the textile usually adopts one or more of amino silicone oil, block silicone oil or fatty amide softening agents, however, the products belong to cationic, and the auxiliaries for the pretreatment, dyeing or printing of the textile contain a large amount of anions (such as dye brightener soaping agent color paste and the like). Therefore, if the preorder process is not completely processed, the residual anionic assistant and cationic silicone oil or soft oil during hand feeling finishing can react, and silicone oil spots and other phenomena can occur on the surface of the textile; in addition, not only residual anionic auxiliary agents are needed, but also the hand feeling auxiliary agents such as silicone oil and the like need to be melted together with the whitening agent or the stiffening agent anionic auxiliary agent for over-shaping during shaping, and at the moment, the materials and the whitening agent or the stiffening agent anionic auxiliary agent can generate anion-cation reaction in a cylinder, so that a large number of silicone oil classes are attached to the surface of the textile; particularly, silicone oil class or soft oil class can be generated when the softening agent is added into a cylinder. However, no silicone softener which meets the requirements of taking the product with good hand feeling and good stability is available in the market. It is therefore necessary to develop an anionic silicone finish to solve this problem. On the other hand, the amino modified silicone oil belongs to a cationic type, and can not be subjected to one-bath with an anionic coloring agent, so that the amino modified silicone oil needs to be treated separately and shaped twice, the process is complex, the cost is increased, and the production efficiency is reduced.
Disclosure of Invention
The invention aims to provide an anionic organosilicon finishing agent and a preparation method thereof, the anionic hand feeling finishing agent can be used with dye of an anionic auxiliary agent in one bath, the treatment efficiency of fabric post-treatment is improved, the production cost is reduced, and the anionic hand feeling finishing agent and the dye of the anionic auxiliary agent both belong to anionic type and can not generate silicon spots and color blocks.
To achieve the above object, the present invention provides an anionic hand feeling finishing agent comprising an additive represented by structural formula I:
wherein the content of the first and second substances,
n is more than or equal to 5, EO is ethylene oxide, PO is propylene oxide, a is more than or equal to 3,b is more than or equal to 4,c is more than or equal to 4,d is more than or equal to 6.
In some embodiments, 20 ≧ a ≧ 3, 30 ≧ b ≧ 4, 30 ≧ c ≧ 4, 20 ≧ d ≧ 6, 30 ≧ n ≧ 5, such that ethylene oxide and propylene oxide are in the appropriate ranges, taking into account hydrophilicity and hand feel, preferably 10 ≧ a ≧ 5, 20 ≧ b ≧ 4, 20 ≧ c ≧ 5, 20 ≧ d ≧ 10.
In some embodiments, the step of preparing the additive comprises:
(1) Reacting primary amine polyether amine with sodium chloroacetate under an alkaline condition to obtain an intermediate A;
(2) Reacting octamethyltetrasiloxane and a hydrogen-containing double-end socket at 30-45 ℃ under the condition of concentrated sulfuric acid serving as a catalyst, filtering a product, and vacuumizing at 140-180 ℃ to prepare an intermediate B;
(3) Reacting the intermediate B treated in the step (2) with allyl epoxy polyether under the condition of chloroplatinic acid catalyst to obtain diepoxy terminated polyether silicone oil;
(4) And reacting the intermediate A with diepoxy terminated polyether silicone oil under the condition of isopropanol to prepare the additive.
In some embodiments, the primary aminated polyether amine has a molecular weight of 400-2000. Illustratively, the weight average molecular weight of the primary aminated polyether amine can be, but is not limited to, 400, 600, 1000, 1600, 1800, 2000, specifically, the primary aminated polyether amine is selected from the group consisting of KL-11, KL-11B, KL-91B, but not limited thereto.
In some embodiments, the alkaline conditions may be, but are not limited to, sodium hydroxide, potassium hydroxide, and the like.
In some embodiments, the allyl epoxy polyether has the following structural formula:
wherein, c is more than or equal to 30 and more than or equal to 4, d is more than or equal to 20 and more than or equal to 6.
In some embodiments, the allyl epoxy polyether has a molecular weight of 500 to 2000. Illustratively, the molecular weight of the allyl epoxy polyether can be, but is not limited to, 500, 1000, 1500, 2000, specifically, the allyl epoxy polyether is selected from APE1000, APE600, APE1500, APEG-1000, but not limited thereto.
In some embodiments, the mass ratio of primary aminated polyetheramine to sodium chloroacetate in step (1) is 5-10.
In some embodiments, the reaction temperature in step (1) is 120-150 ℃, and illustratively, the reaction temperature may be, but is not limited to, 120 ℃, 130 ℃, 140 ℃, 150 ℃.
In some embodiments, in step (2), the mass ratio of octamethyltetrasiloxane to hydrogen-containing double head is from 0.5 to 2.
In some embodiments, in step (3), the mass ratio of intermediate B to allyl epoxy polyether is 5 to 10.
In some embodiments, the reaction temperature in step (3) is less than 85 ℃, preferably less than 85 ℃, and more preferably 75 to 80 ℃.
In some embodiments, the reaction temperature in step (4) is 80-120 ℃, and illustratively, the reaction temperature may be, but is not limited to, 80 ℃, 90 ℃, 100 ℃, 110 ℃, 120 ℃.
In some embodiments, in step (4), the mass ratio of intermediate a to diepoxy terminated polyether silicone oil is from 100.
In some embodiments, the present invention provides a preparation route of an additive, but is not limited to the preparation route, the preparation route is as follows:
step (1)
Step (2):
and (3):
setting up
Namely, it is
And (4):
in some embodiments, the anionic hand feel finish further comprises fatty alcohol polyoxyethylene ether, alcohol ether carboxylate, glacial acetic acid, glycerol, water. The additive is emulsified by the fatty alcohol-polyoxyethylene ether and compounded with the alcohol ether carboxylate and the glycerol, so that the product is smooth and plump in hand feeling.
In some embodiments, the water-based paint comprises, by weight, 10-30 parts of an additive, 5-20 parts of fatty alcohol-polyoxyethylene ether, 10-20 parts of alcohol ether carboxylate, 1-10 parts of glacial acetic acid, 1-10 parts of glycerol and 30-60 parts of water.
In some embodiments, 20-40 parts of the brightener 4,4 '-bis (4,6-dianilinotriazinyl-2-amino) stilbene-2,2' -disulfonic acid sodium salt is also included. The whitening agent belongs to anions, and the additive also belongs to anions, so that the whitening agent can be directly added into the finishing agent containing the additive to realize one-bath use, the after finishing of the textile is simpler, the soft hand feeling and dyeing of the textile can be completed in one step, the production efficiency can be effectively improved, the enterprise cost is reduced, the process is simplified, and the whitening agent and the finishing agent both belong to anions, so that the situations of color spots and color blocks can be avoided.
In some embodiments, the fatty alcohol polyoxyethylene ether has the formula RO (CH) 2 CH 2 O) n H, R is generally saturated or unsaturated C 12 -C 18 N =15-20, for example, the fatty alcohol polyoxyethylene ether may be peregal O, but is not limited thereto.
Correspondingly, the invention also provides a preparation method of the anionic hand feeling finishing agent, which comprises the following steps:
the raw materials of the anionic hand feeling finishing agent are stirred uniformly in one bath.
Specifically, 10-30 parts of additive, 5-20 parts of fatty alcohol-polyoxyethylene ether, 10-20 parts of alcohol ether carboxylate, 1-10 parts of glacial acetic acid, 1-10 parts of glycerol, 30-60 parts of water and 5-15 parts of whitening agent 4,4 '-bis (4,6-diphenylamino triazinyl-2-amino) stilbene-2,2' -disulfonic acid sodium salt are stirred uniformly in the same bath to prepare the anionic hand feeling finishing agent.
The invention has the following beneficial effects:
the anionic hand feeling finishing agent comprises an additive shown as a structural formula I, wherein the additive contains an anionic structure after being ionized in water,
the anionic hand feeling finishing agent can be used together with anionic dye in a bath, soft hand feeling and dyeing of textiles can be finished in one step, production efficiency can be effectively improved, enterprise cost is reduced, process simplification is achieved, the anionic hand feeling finishing agent and the anionic dye belong to anionic type, and color spots and color blocks cannot appear. Meanwhile, the two positions of the additive of the anionic hand feeling finishing agent contain ethylene oxide, the hydrophilic performance is good, the two positions contain propylene oxide, the hand feeling of the textile fabric can be improved, and particularly, carboxyl in the additive can be deeply combined with hydroxyl on the surface of fabric fiber, so that the product is endowed with soft, smooth and plump hand feeling.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
An anionic hand feeling finishing agent comprises, by weight, 15 parts of an additive, 15 parts of peregal O, 12 parts of alcohol ether carboxylate, 5 parts of glacial acetic acid, 10 parts of glycerol, 40 parts of water, 5 parts of 4,4 '-bis (4,6-dianilinotriazinyl-2-amido) stilbene-2,2' -disulfonic acid sodium salt,
the preparation method of the additive comprises the following steps:
(1) Adding 50g of primary amine-modified polyetheramine Koron KL-91B and 10g of sodium chloroacetate into a reaction bottle, adding sodium hydroxide, and reacting at 140 ℃ for 24 hours to obtain an intermediate A;
(2) Sequentially adding 100g of octamethyltetrasiloxane and 1g of hydrogen-containing double-end socket into a reaction bottle, adding a proper amount of concentrated sulfuric acid as a catalyst, reacting for 24 hours at the temperature of 40 ℃, filtering a product, and vacuumizing for 2 hours at the temperature of 160 ℃ to prepare an intermediate B;
(3) Adding 50g of the intermediate B treated in the step (2) and 10g of allyl epoxy polyether APEG-1000 into a reaction bottle, adding appropriate isopropanol, reacting for 8 hours at the temperature of 80 ℃ under the condition of chloroplatinic acid catalyst to obtain diepoxy terminated polyether silicone oil;
(4) And (3) reacting 20g of the intermediate A with 100g of diepoxy terminated polyether silicone oil for 10 hours under the condition of isopropanol at the temperature of 100 ℃ to obtain the additive.
The preparation method of the anionic hand feeling finishing agent comprises the following steps:
the anionic hand feeling finishing agent is prepared by uniformly stirring an additive, peregal O, alcohol ether carboxylate, glacial acetic acid, glycerol, water and 4,4 '-bis (4,6-diphenylamine-triazinyl-2-amino) stilbene-2,2' -disulfonic acid sodium salt in one bath.
Example 2
An anionic hand feeling finishing agent comprises, by weight, 20 parts of an additive, 18 parts of peregal O, 15 parts of alcohol ether carboxylate, 5 parts of glacial acetic acid, 5 parts of glycerol, 50 parts of water, 6 parts of 4,4 '-bis (4,6-dianilinotriazinyl-2-amido) stilbene-2,2' -disulfonic acid sodium salt,
wherein the additives are the same as in example 1 and are not described in detail herein.
The preparation process is referred to example 1 and is not described in detail here.
Example 3
An anionic hand feeling finishing agent comprises, by weight, 25 parts of an additive, 20 parts of peregal O, 20 parts of alcohol ether carboxylate, 8 parts of glacial acetic acid, 3 parts of glycerol, 45 parts of water, 8 parts of 4,4 '-bis (4,6-dianilinotriazinyl-2-amido) stilbene-2,2' -disulfonic acid sodium salt,
wherein the additives are the same as in example 1 and are not described in detail herein.
The preparation process is referred to example 1 and is not described in detail here.
Comparative example 1
This comparative example is essentially the same as example 1, except that: the alcohol ether carboxylate is not contained in comparative example 1, but contained in example 1, and the rest is the same as example 1, and will not be described in detail.
The anionic hand feeling finishing agents obtained in examples 1 to 3 and comparative example 1 were used for post-finishing of cotton fabrics, and then performance tests were performed, and the results are shown in table 1.
The blank was run with water.
Hydrophilicity: hydrophilicity was judged by the static drip method by dropping 1 drop of water from 1cm to the fabric using a standard dropper (25 drops/mL) and taking the time for complete absorption of the water drop. The shorter the time, the better the hydrophilicity.
Hand feel test performance: and (3) a physical hand feeling evaluation method is adopted, the finished cloth sample is cooled and remoistened, and the original cloth hand feeling is rated as 1 point through comprehensive evaluation of multiple qualified hand feeling evaluation professionals from the aspects of smoothness, softness, filling power and the like, the hand feeling evaluation is preferably rated as 5 points, and the average value is taken.
And (3) stability testing: centrifuging and storing the anionic hand feeling finishing agent for 24 hours to see whether the layering phenomenon occurs or not; the centrifugation condition is 3000r/min,30min.
And (4) appearance observation, namely observing whether the color of the treated cotton fiber fabric is whitened or not by naked eyes.
TABLE 1 test results
From the test results in Table 1, it can be seen that the hand feeling of the blank sample is 1 point, the hand feeling of examples 1 to 3 is greatly improved, and the anionic hand feeling finishing agent has good hydrophilicity and stability, can be used in one bath, and does not generate silicon spots and color blocks. The absence of alcohol ether carboxylate in comparative example 1 resulted in a decrease in both hand and hydrophilicity.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. An anionic hand treatment comprising an additive of formula I:
wherein, the first and the second end of the pipe are connected with each other,
n is more than or equal to 5, EO is ethylene oxide, PO is propylene oxide, a is more than or equal to 3,b is more than or equal to 4,c is more than or equal to 4,d is more than or equal to 6.
2. The anionic hand feeling finishing agent according to claim 1, wherein 20. Gtoreq.a.gtoreq.3, 30. Gtoreq.b.gtoreq.4, 30. Gtoreq.c.gtoreq.4, 20. Gtoreq.d.gtoreq.6, 30. Gtoreq.n.gtoreq.5.
3. The anionic hand treatment of claim 1, wherein the additive is prepared by a process comprising:
(1) Reacting primary amine polyether amine with sodium chloroacetate under an alkaline condition to prepare an intermediate A;
(2) Reacting octamethyltetrasiloxane and a hydrogen-containing double-end socket at 30-45 ℃ under the condition of concentrated sulfuric acid serving as a catalyst, filtering a product, and vacuumizing at 140-180 ℃ to prepare an intermediate B;
(3) Reacting the intermediate B treated in the step (2) with allyl epoxy polyether under the condition of chloroplatinic acid catalyst to obtain diepoxy terminated polyether silicone oil;
(4) And reacting the intermediate A with diepoxy terminated polyether silicone oil under the condition of isopropanol to prepare the additive.
4. The anionic hand treatment of claim 3, wherein the primary aminated polyetheramine has a molecular weight of 400 to 2000.
5. The anionic hand treatment of claim 3, wherein the alkaline condition is one of sodium hydroxide and potassium hydroxide.
6. The anionic hand treatment of claim 3, wherein the allyl epoxy polyether has a molecular weight of 500 to 2000.
7. The anionic hand treatment of claim 1, further comprising fatty alcohol polyoxyethylene ether, alcohol ether carboxylate, glacial acetic acid, glycerol and water.
8. The anionic hand feeling finishing agent according to claim 7, which comprises, by weight, 10-30 parts of an additive, 5-20 parts of fatty alcohol-polyoxyethylene ether, 10-20 parts of alcohol ether carboxylate, 1-10 parts of glacial acetic acid, 1-10 parts of glycerol and 30-60 parts of water.
9. The anionic hand treatment of claim 8 further comprising 5 to 15 parts of 4,4 '-bis (4,6-dianilinotriazinyl-2-amido) stilbene-2,2' -disulfonic acid sodium salt.
10. A process for preparing an anionic hand treatment according to any one of claims 1 to 9, characterised in that it comprises the steps of:
and uniformly stirring all the raw materials of the anionic hand feeling finishing agent in the same bath to prepare the anionic hand feeling finishing agent.
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