Nitrogen oxide-resistant fabric improver and preparation method thereof

Abstract

The invention discloses a fabric nitrogen oxide resistance improver and a preparation method thereof, and aims to provide an improver which can improve the nitrogen oxide resistance of cotton fabrics and has good durability, the structural formula is as follows: # imgabs0 #, and n = 1-2500; belongs to the technical field of applied chemistry.

Description

Technical Field

[0001] The invention relates to a nitrogen oxide resistance improving agent for fabrics, in particular to a nitrogen oxide resistance improving agent for fabrics targeting reactive dyes / direct dyes / sulfur dyes and the like. The invention also discloses a preparation method of the improving agent, belonging to the technical field of applied chemistry. Technical Background

[0002] In recent years, in order to save energy and reduce emissions and pollution to the environment, many dyeing factories have adopted natural gas setting machines to replace traditional setting machines that use coal or fuel as energy. However, as a result, the combustion byproduct nitrogen oxides have a significant negative impact on textiles. Nitrogen oxides can destroy the dye structure, cause the fabric color to fade, and greatly affect the appearance of the fabric. We all know that the normal atmosphere also contains about 0.01 to 0.02 ppm of nitrogen oxides, and the automobile exhaust is even higher, up to about 500 ppm.

[0003] As early as the beginning of the 20th century, American scientists pointed out that nitrogen oxides in the air, especially in automobile exhaust, would cause dyes, especially anthraquinone dyes containing amino groups, to fade or change color. The main reactions are as follows:

[0004] (a) Reaction with primary amino groups in dyes

[0005]

[0006] (b) Reaction with secondary amine groups in dyes

[0007]

[0008] Therefore, improving the resistance of fabrics to nitrogen oxide damage has become an urgent issue. There are few reports on the resistance of fabrics to nitrogen oxides. Although there are some products on the market that claim to improve the resistance of fabrics to nitrogen oxides, most of them do not disclose the product structure. Moreover, according to our research, it is not washable and the effect is almost gone after multiple washings. Summary of the invention

[0009] Therefore, the object of the present invention is to provide a kind of improving agent which can improve the nitrogen oxide resistance of cotton fabric and has good durability.

[0010] Another object of the present invention is to provide a method for preparing the enhancer, which has readily available raw materials and a simple process.

[0011] To this end, the first technical solution provided by the present invention is as follows:

[0012] A fabric nitrogen oxide resistance enhancing agent having the following structural formula (I):

[0013]

[0014] Among them, n=1~2500.

[0015] The second technical solution provided by the present invention is a method for preparing the fabric nitrogen oxide resistance enhancing agent described in the first technical solution, which comprises the following steps in sequence:

[0016] 1) Add water and polyethyleneimine into a four-necked flask, start stirring, condense water and nitrogen, and heat in a water bath to 60-70°C;

[0017] 2) When the temperature in the reactor reaches 60-70°C, epichlorohydrin is added dropwise and the addition is completed within 3-5 hours;

[0018] 3) After the epichlorohydrin is added dropwise, the temperature is raised to 75-85°C and kept warm for 2-4 hours;

[0019] 4) Cooling to room temperature, discharging the material, and filtering to obtain a viscous liquid which is the smoke fastness enhancer.

[0020] Furthermore, in the preparation method of the above-mentioned physical nitrogen oxide resistant enhancing agent, the four-necked flask is equipped with nitrogen protection, a condenser, a thermometer and a stirring device.

[0021] According to the method for preparing a nitrogen oxide resistant enhancing agent according to claim 1, the stirring speed in step 1) is 600 rpm.

[0022] Furthermore, in the preparation method of the above-mentioned physical nitrogen oxide resistance enhancing agent, the filtration adopts a 200-mesh filter.

[0023] Compared with the prior art, the present invention has the following advantages:

[0024] 1. The fabric nitrogen oxide resistance enhancing agent provided by the present invention has abundant -NH groups, which can play a very good role in nitrogen oxide corrosion resistance;

[0025] 2. The fabric nitrogen oxide resistance enhancer provided by the present invention contains active groups of chlorine and hydroxyl, which can be combined with fibers and dyes to form stable covalent bonds. In addition, the -NH group in its structure can also form hydrogen bonds with dyes and fibers. At the same time, the enhancer is a polymer structure and can form a polymer film on the surface of the fabric. All these factors make the enhancer effect able to withstand multiple washings, and the product has good durability;

[0026] 3. The fabric nitrogen oxide resistance enhancing agent provided by the present invention has readily available raw materials and a simple process. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] Figure 1 This is the FTIR spectrum of a fabric nitrogen oxide resistance enhancing agent provided in Example 3. DETAILED DESCRIPTION

[0028] The following is a clear and complete description of the technical solutions implemented in the present invention. Obviously, the described embodiments are only the main test processes of the present invention. For process parameters or conditions not specifically specified, conventional techniques can be used.

[0029] Example 1

[0030] The present invention provides a fabric nitrogen oxide resistance enhancing agent, the structural formula of which is as follows:

[0031]

[0032] Where: n = 2

[0033] The preparation of the fabric resistant nitrogen oxide resistant enhancing agent comprises the following steps in sequence:

[0034] 1) Add 20g of water and 20g of polyethyleneimine into a 100ml four-necked flask (with nitrogen protection, condenser, thermometer and stirring device), start stirring (speed 600rpm), condense water and nitrogen, start water bath heating equipment, and heat to 70°C;

[0035] 2) When the temperature in the reactor reaches 70°C, epichlorohydrin is added dropwise. 20.35 g of epichlorohydrin is added dropwise within four hours. If the temperature exceeds 70°C during this period, ice cubes can be added to the water bath to prevent overheating and gelation;

[0036] 3) After the epichlorohydrin is added, the temperature is raised to 85°C and kept warm for 3 hours;

[0037] 4) Cool down to room temperature, discharge the material, and filter out possible impurities with a 200-mesh sieve to obtain a yellow viscous liquid, which is the smoke fastness enhancer.

[0038] Example 2

[0039] The present invention provides a smoke fastness improving agent, the structural formula of which is:

[0040]

[0041] Where: n = 56

[0042] The preparation of the fabric nitrogen oxide resistance enhancing agent comprises the following steps in sequence:

[0043] 1) Add 50g water and 50g polyethyleneimine into a 250ml four-necked flask (with nitrogen protection, condenser, thermometer and stirring device), start stirring (speed 600rpm), condense water and nitrogen, start water bath heating equipment, and heat to 70°C;

[0044] 2) When the temperature in the reactor reaches 70°C, epichlorohydrin is added dropwise. 46 g of epichlorohydrin is added dropwise within four hours. If the temperature exceeds 70°C during this period, ice cubes can be added to the water bath to prevent overheating and gelation;

[0045] 3) After the epichlorohydrin is added, the temperature is raised to 70°C and kept warm for 3 hours;

[0046] 4) Cool down to room temperature, discharge the material, and filter possible impurities with a 200-mesh sieve to obtain a brown-yellow viscous liquid, which is the fabric nitrogen oxide resistance enhancer.

[0047] Example 3

[0048] The present invention provides a fabric nitrogen oxide resistance enhancing agent, the structural formula of which is:

[0049]

[0050] Where: n = 1690

[0051] The preparation of the fabric nitrogen oxide resistance enhancing agent comprises the following steps in sequence:

[0052] 1) Add 60g water and 60g polyethyleneimine into a 250ml four-necked flask (with nitrogen protection, condenser, thermometer and stirring device), start stirring (speed 600rpm), condense water and nitrogen, start water bath heating equipment, and heat to 70°C;

[0053] 2) When the temperature in the reactor reaches 60°C, epichlorohydrin is added dropwise. 55 g of epichlorohydrin is added dropwise within four hours. If the temperature exceeds 70°C during this period, ice cubes can be added to the water bath to prevent overheating and gelation;

[0054] 3) After the epichlorohydrin is added, the temperature is raised to 80°C and kept warm for 4 hours;

[0055] 4) Cool down to room temperature, discharge the material, and filter possible impurities with a 200-mesh sieve to obtain a brown to red viscous liquid, which is the fabric nitrogen oxide resistance enhancer.

[0056] The FTIR spectrum of the agent is shown in Figure 1 ,from Figure 1 It can be seen that 3250-3400 cm~1 is the stretching vibration peak of NH and OH, 1450-1650 cm~1 is the bending vibration peak of NH, the peaks at 2800 cm~1, 2950 cm~1 and 1100 cm~1, 1300 cm~1 are the vibration absorption peaks of methylene, and 750-800 cm~1 is the absorption peak of C~Cl.

[0057] In order to demonstrate the effect of the technical solution provided by the present application, the performance test process and data of the fabric nitrogen oxide resistance enhancing agent provided in Examples 1 to 3 are given below:

[0058] The application formula process is as follows:

[0059] Test fabric: knitted cotton fabric dyed and fixed with reactive turquoise blue dye (0.5%)

[0060] Test process: any one of hydrazides and piperazines in Examples 1 to 3 is rolled onto the above-mentioned test cloth at 10 g / l using a setting machine, set at high temperature of 150° C. for 2 minutes, and then cooled to room temperature for nitrogen oxide resistance test.

[0061] 1. Resistance to nitrogen oxides is carried out according to ISO 105~G01 method; the results are shown in Table 1:

[0062] Table 1

[0063]

[0064] As can be seen from Table 1, compared with traditional nitrogen oxide-resistant products (hydrazides and piperazines), Examples 1 to 3 of the present invention have slightly better fastness before washing, and the advantage is obvious after washing 5 times, indicating that the nitrogen oxide-resistant fabric enhancing agent provided by the present invention has abundant -NH groups and can play a very good effect; and because the structure contains active group chlorine, and the enhancing agent is a polymer structure, it can be combined with fibers and dyes to form stable covalent bonds / hydrogen bonds and film-forming effects, the nitrogen oxide resistance effect can withstand multiple washings, and the product has good durability.

Claims

1. A fabric nitrogen oxide resistance enhancing agent, characterized in that: It has the following structural formula (I): Among them, n=1~2500.

2. The method for preparing the nitrogen oxide resistance enhancing agent for fabrics according to claim 1, characterized in that: The steps are as follows: 1) Add water and polyethyleneimine into a four-necked flask, start stirring, condense water and nitrogen, and heat in a water bath to 60-70°C; 2) When the temperature in the reactor reaches 60-70°C, epichlorohydrin is added dropwise and the addition is completed within 3-5 hours; 3) After the epichlorohydrin is added dropwise, the temperature is raised to 75-85°C and kept warm for 2-4 hours; 4) Cooling to room temperature, discharging, and filtering to obtain a viscous liquid, which is a smoke fastness enhancer; The mass ratio of water, polyethyleneimine and epichlorohydrin is 20-60:20-60:20.35-55.

3. The method for preparing the nitrogen oxide resistance enhancing agent for fabrics according to claim 2, characterized in that: The four-necked flask was equipped with nitrogen protection, condenser, thermometer and stirring device.

4. The method for preparing the nitrogen oxide resistance enhancing agent for fabrics according to claim 2, characterized in that: The stirring speed in step 1) is 600 rpm.

5. The method for preparing the nitrogen oxide resistance enhancing agent for fabrics according to claim 2, characterized in that: The filtration adopts a 200-mesh filter.

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