JP2014156549A - Flame-retardant coating agent and flame-retardant processed fabric - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a flame-retardant coating agent for a polyester fiber fabric using a halogen-free compound as a flame retardant, having a sufficient flame retardance, and simultaneously accompanied by scarce water spots on a processed fabric; and a flame-retardant processed fabric to which the flame-retardant coating agent is applied.SOLUTION: The provided flame-retardant coating agent comprises: a crosslinked acrylic resin; aluminum trisdiethylphosphinate, aluminum trismethylethylphosphinate, or aluminum trisdiphenylphosphinate as a flame retardant component; a urethane association-type thickener; acetylene glycol; and a compatibility enhancer. Non-volatile component ratios, after drying at 150°C, of the flame retardant component, urethane association-type thickener, and acetylene glycol with respect to 1.0 of the crosslinked acrylic resin are respectively 0.3-2.0, 0.05-0.2, and 0.001-0.02. The compatibility enhancer has a boiling point of 80 to 150°C and is mixed, as a component not remaining after drying, at a ratio of 0.01-0.2 with respect to 1.0 of the non-volatile component of the crosslinked acrylic resin. A flame-retardant processed fabric to which the flame-retardant coating agent is applied is also provided.

Description

  The present invention relates to a coating agent for subjecting a textile product to flame retardancy and a fabric flame retarded with the coating agent.

  Conventionally, halogen-based compounds such as decabromodiphenyl ether have been used in flame-retardant processing for polyester fiber fabrics, but when halogen-based compounds are used, harmful halogenated gases are generated when the polyester fiber fabric burns, and the environment There are problems such as harmful effects on Therefore, it has been found that an organophosphorus compound has good flame retardancy as a flame retardant component that is replaced by a halogen compound. (Patent Document 1)

  However, many of the organic phosphorus flame retardants have a problem in water resistance, and there is a problem that a part of the flame retardant elutes when warm water or water is applied to the polyester fabric. Also, ammonium polyphosphate, which is often used as a flame retardant coating agent, has a problem of water resistance. (Patent Document 2)

  On the other hand, various studies have been conducted on compositions used in combination with flame retardants. Patent Document 3 is an invention of a resin composition for a backing material (back coating agent) used for interior materials such as automobiles. In this document, a resin composition containing an internal cross-linkable resin having a specific chemical structure and a flame retardant has a delayed flame propagation due to carbonization of the resin during combustion, that is, has a slow flame retardancy. It is disclosed that it has a high effect on the production of flame retardant fabrics.

  The above-mentioned document does not mention properties other than slow-flammability. However, in order to put the flame-retardant processed fabric into practical use, various requirements other than flame retardancy (slow flame retardancy) are required. In particular, in the case of a flame-retardant processed fabric, a ring-shaped wrinkle (with wrinkles) is caused after warm water or water is applied to the fabric due to the influence of components such as a flame retardant, a compatibility improver, a thickener, and a binder. ) Is a problem, and there has been a demand for a flame retardant that does not cause wrinkles.

  In particular, recent interior materials for vehicles are lighter in weight due to demands for weight reduction, and thin fabrics are increasing. However, there is a problem that such fabrics are prone to wrinkles. There is a demand for flame retardant processing agents that are less susceptible to wrinkling and that can impart sufficient flame retardancy.

Japanese Patent Publication No.53-8840 JP 2006-28488 A JP 2007-269999 A

  In view of the above, the present invention provides a flame retardant coating agent for polyester fiber fabrics that uses a dehalogenated compound as a flame retardant and has sufficient flame retardancy and at the same time is less likely to cause wrinkles in processed fabrics. Let it be an issue.

  The present inventors have found that the use amount of a flame retardant can be reduced by using a cross-linked acrylic resin as a binder used in combination with the flame retardant. Furthermore, by reducing the amount of flame retardant used, the amount of high boiling point dispersant essential for dispersing the flame retardant is reduced, and at the same time, a compatibility improver having a lower boiling point than the drying temperature after coating is used in combination. Thus, the present inventors have found that a flame retardant coating agent that is excellent in flame retardancy and has no problem of generation of wrinkles can be obtained in practice, and the present invention has been completed.

  That is, the present invention is a flame retardant coating agent comprising a crosslinkable acrylic resin, an alkyl phosphate metal salt, a urethane associative thickener, acetylene glycol and a compatibility improver, and has a non-volatile component ratio after drying at 150 ° C. The alkyl phosphate metal salt is 0.3 to 2.0, the urethane-associated thickener is 0.05 to 0.2, and the acetylene glycol is 0.001 to 0.02 with respect to the cross-linked acrylic resin 1.0. The compatibility improver has a boiling point of 80 to 150 ° C. and does not remain after drying, and is blended at a ratio of 0.01 to 0.2 with respect to the non-volatile component 1.0 of the cross-linked acrylic resin. The present invention relates to a flame retardant coating agent.

  According to the flame retardant coating agent of the present invention, it is possible to obtain a flame retardant processed fabric having sufficient flame retardancy and at the same time, having no problem of generation of wrinkles in a fabric treated with the flame retardant coating agent. Can do.

The present invention further contains aluminum hydroxide, and the aluminum hydroxide has a non-volatile component ratio after drying at 150 ° C. of 0.9 to 2.5 with respect to the cross-linked acrylic resin 1.0. It is related with the said flame-retardant coating agent characterized by being mix | blended.
Aluminum hydroxide is considered to have a function as a flame retardant aid, and the addition of aluminum hydroxide makes it possible to reduce the amount of alkyl phosphate metal salt used, and thus the high boiling point that causes wrinkles. The amount of dispersant used can be reduced, and the occurrence of wrinkles can be further suppressed.

Furthermore, the present invention relates to the flame retardant coating agent described above, wherein the gel fraction of the cross-linked acrylic resin and the weight residual ratio after combustion are 80% or more.
By using a resin having a gel fraction and a weight residual ratio after combustion of 80% or more, it is possible to obtain a coating agent that is less prone to wrinkle and can provide a fabric excellent in flame retardancy.

In the present invention, the compatibility improver is one or more compatibility improvers selected from the group consisting of isopropyl alcohol, normal propyl alcohol, methyl cellosolve, ethyl cellosolve, isopropyl cellosolve and tertiary butyl cellosolve. The flame retardant coating agent is characterized by the above.
These compatibility improvers have a boiling point lower than the drying temperature after coating. According to the flame retardant coating agent containing these compatibility improvers, it is possible to reliably obtain a fabric that is excellent in flame retardancy and does not generate wrinkles, and flame retardant processing is performed using conventional equipment and methods. This can be done at a practical cost.

Furthermore, this invention relates to the flame-retardant processed fabric processed with one of the said flame-retardant coating agents.
The flame-retardant processed fabric of the present invention is excellent in flame retardancy, has no generation of wrinkles and is excellent in quality stability, and thus has extremely high practicality and is widely used for applications requiring flame retardancy. be able to.

The flame-retardant processed fabric of the present invention is preferably a fabric having a flame-retardant coating only on one side of a polyester fabric having a basis weight of 250 to 400 g / m ² and a thickness of 1.5 mm or less.
In general, a fabric with a light basis weight is likely to be wrinkled, and it has been difficult to subject such a fabric to flame-retardant processing by single-side coating (back coating). However, the fabric of the present invention has the above-mentioned basis weight. Also has good flame retardancy and no wrinkles. This fabric with flame retardant processed only on one side (back side) is highly safe because the user does not touch the coating layer directly, and it is possible to make it a material that takes advantage of the original texture and aesthetics of the fabric. is there.

  The flame-retardant coating agent of the present invention is characterized in that it can impart sufficient flame retardancy to the fabric, and at the same time, the occurrence of wrinkles in the treated fabric is extremely small, or there is no occurrence of wrinkles, In particular, it can be effectively used for polyester fabrics that are vehicle interior materials, especially vehicle interior materials that are light in weight and light in color.

  The flame retardant coating agent of the present invention contains a cross-linked acrylic resin that mainly functions as a binder. The cross-linked acrylic resin refers to a resin that undergoes a cross-linking reaction when heated. For example, “slow-flammable resin composition” described in JP-A-2007-269999 can be used. Since these resins tend to carbonize without being melted during combustion, they are effective in reducing the combustion rate. Such a resin may be referred to as a carbonized acrylic resin.

  Specific examples of the crosslinkable acrylic resin include an internal crosslinkable acrylic resin having an epoxy group and a carboxyl group. By polymerizing a carboxyl group-containing monomer or an epoxy group-containing monomer, the resin can contain a carboxyl group and an epoxy group.

Examples of such a resin include a resin mainly composed of a (meth) acrylic polymer obtained by polymerizing a (meth) acrylic monomer. For example, the polymer which copolymerized the monomer which has (meth) acrylic-acid alkylester, the monomer which has a carboxyl group, and the epoxy group is mentioned.
Examples of the monomer having a carboxyl group include (meth) acrylic acid, itaconic acid, maleic acid, and maleic anhydride, and examples of the monomer having an epoxy group include glycidyl (meth) acrylate. The carboxyl group contained in the resin may be neutralized with an organic amine compound or the like.

  The crosslinked acrylic resin also preferably has a gel fraction and a weight residual ratio after combustion of 80% or more. The gel fraction is an index representing the degree of crosslinking of the polymer, and the calculation method is shown in the examples described later. Further, the weight residual ratio after combustion represents the degree of carbonization of the resin during combustion, and the larger the number, the greater the degree of carbonization. The calculation method is shown in the examples described later.

  As the cross-linked acrylic resin, a commercially available fiber binder containing the resin as described above can be appropriately selected and used. For example, Rikabond (manufactured by Chuo Rika Co., Ltd.) can be used.

  The flame retardant component contained in the coating agent of the present invention is an alkyl phosphate metal salt. Examples of the alkyl phosphate metal salt include aluminum trisdiethylphosphinate (manufactured by Clariant), aluminum trismethylethylphosphinate (manufactured by Clariant), and aluminum trisdiphenylphosphinate (manufactured by Clariant).

  The coating agent of the present invention contains a urethane associative thickener as a thickener. As the urethane associative thickener, a commercially available urethane associative thickener, for example, biscon (manufactured by Shin-Nakamura Chemical Co., Ltd.) can be used.

  The coating agent of the present invention contains acetylene glycol. Acetylene glycol is believed to function as a dispersant for the flame retardant component. As acetylene glycol, commercially available surfinol (manufactured by Nissin Chemical Co., Ltd.), orphine (manufactured by Nissin Chemical Co., Ltd.) and the like can be used. In this specification, acetylene glycol includes acetylene glycol and acetylene glycol derivatives. Examples of the acetylene glycol derivative include an acetylene glycol EO adduct obtained by adding 10 to 80% of ethylene oxide (EO) to acetylene glycol.

  The above cross-linked acrylic resin, alkyl phosphate metal salt, urethane associative thickener and acetylene glycol are processed into a non-volatile component after the flame retardant coating agent is processed into a fabric and subjected to a drying step (for example, about 150 ° C. for about 3 minutes). As a component remaining in the fabric. The ratio of these non-volatile components is 0.3 to 2.0 for the alkyl phosphate metal salt with respect to the cross-linked acrylic resin 1.0. When the content ratio of the alkyl phosphate metal salt is less than 0.3, the flame retardancy is insufficient, and when the content ratio is more than 2.0, generation of wrinkles is observed in the treated fabric. The urethane associative thickener is contained at a ratio of 0.05 to 0.2 with respect to 1.0 of the cross-linked acrylic resin. If the urethane associative thickener is less than 0.05, the thickening is not sufficient, so that the flame retardant coating agent penetrates to the fabric surface, and if it exceeds 0.2, the viscosity is high and the coatability is poor. Acetylene glycol is contained at a ratio of 0.001 to 0.02 with respect to 1.0 of the cross-linked acrylic resin. When the amount of acetylene glycol is less than 0.001, the metal alkyl phosphate cannot be sufficiently dispersed in the coating agent. When the amount is more than 0.02, the fabric is wrinkled.

Furthermore, the coating agent of the present invention contains a compatibility improver as a component that does not substantially remain on the fabric after the drying step. The compatibility improver is an organic solvent component having both hydrophilicity and hydrophobicity, which has a function of stably dispersing components such as an alkyl phosphate metal salt together with acetylene glycol in a coating agent.
As the compatibility improver, one having a boiling point of 80 to 150 ° C. is used. However, a compatibility improver having a boiling point lower than 80 ° C. volatilizes during transportation and storage, and the quality stability of the coating agent is not sufficient. There is a possibility that the compatibility improver having a boiling point higher than 150 ° C. is not preferable because it is not sufficiently removed in the drying step and causes wrinkles.

  Examples of the compatibility improver include isopropyl alcohol, normal propyl alcohol, methyl cellosolve, ethyl cellosolve, isopropyl cellosolve, and tertiary butyl cellosolve. Among these, one type or a combination of two or more types can be used. Moreover, it is also possible to use together the agent which has a compatibility improvement effect other than these, for example, surfactant and a solvent may be included. The compatibility improver is preferably contained at a ratio of 0.01 to 0.2 with respect to the nonvolatile component of the cross-linked acrylic resin. When the compatibility improver is less than 0.01, the dispersibility of the coating agent becomes insufficient, resulting in poor quality stability, and from the viewpoint of reducing volatile components, it is preferably within 0.2.

  The coating agent of the present invention preferably further contains aluminum hydroxide. As aluminum hydroxide, ALMORIX B-325 (manufactured by Armorix), ALMORIX B-316 (manufactured by Armorix), ALMORIX B-315 (manufactured by Armorix), ALMORIX B-313 (manufactured by Armorix), ALMORIX B-312 (manufactured by Armorix), ALMORIX B-309 (manufactured by Armorix), ALMORIX B-303 (manufactured by Armorix), Heidilite H-21 (manufactured by Showa Denko), Heidilite H-31 ( Showa Denko), Heidilite H-32 (Showa Denko) Heidilite H-42 (Showa Denko), Heidilite H-42M (Showa Denko) and the like can be used. It is preferable that aluminum hydroxide is contained in a ratio of 0.9 to 2.5 with respect to the non-volatile component 1.0 of the cross-linked acrylic resin. If it is less than 0.9, the contribution to flame retardancy becomes insufficient, and if it exceeds 2.5, the solid content tends to fall off.

  In addition, functional agents such as antibacterial agents, deodorants, and antistatic agents may be added to the coating agent as needed, and process improvers such as antifoaming agents, leveling agents, and preservatives may be added. Is possible.

  The flame retardant coating agent of the present invention is provided as an aqueous dispersion in which the above-described components are blended. The amount of water contained in the flame retardant coating agent is not particularly limited as long as each component can be stably dispersed. Depending on the coating method, for example, the non-volatile component of the cross-linked acrylic resin may be 2.0 to 5.0. If it is less than 2.0, the coating amount cannot be finely controlled, and if it is more than 5.0, moisture permeation may occur on the surface of the fabric during processing.

  The fabric of this invention is a fabric which has the flame retardance to which the said coating agent was provided. As the fabric, a fabric made of synthetic fibers such as nylon, polyester, polyurethane, polyamide, rayon, acrylic, a fabric made of natural fibers such as cotton, wool, hemp, silk, etc., and these synthetic fibers and / or natural fibers are blended or mixed. Although there are woven fabrics and the like, fabrics made of polyester fibers or fabrics containing polyester fibers are preferred. In this specification, the polyester fabric includes a fabric made of a polyester fiber alone and a fabric made of a fiber using a combination of a polyester fiber and another fiber.

The fabric may be a woven fabric, a knitted fabric, or a non-woven fabric, and the basis weight may be, for example, 250 to 400 g / m ² . The color of the fabric is not particularly limited, but it may be a dark color or a light-colored fabric (for example, one having a lightness measured according to JIS Z8729 of 40 or more).

The coating amount of the coating agent to the fabric is not particularly limited as long as it has sufficient flame retardancy and generation of wrinkles is suppressed, but it is applied so that the coating amount after drying is 30 to 130 g / m ^2. 40 to 100 g / m ² is more preferable.
Conventionally, a light-colored fabric to which a flame retardant coating agent has been added is prone to wrinkles and has a problem because it is easily noticeable. However, a fabric using the coating agent of the present invention has less wrinkles and has an arbitrary thickness. And a fabric having a color can be selected as desired.

The fabric of the present invention is preferably provided with a flame retardant only on one side of the fabric, and in particular, the flame retardant is coated only on the back side of the fabric. The coating method is not particularly limited and can be performed by a known method. For example, a predetermined amount of a flame retardant coating agent is applied onto a fabric by a gravure roll coater, knife coater, reverse roll coater, and the like, and then dried. Thus, a fabric imparted with flame retardancy can be obtained.
It is preferable to perform a drying process at about 120-160 degreeC. If the drying temperature greatly exceeds 150 ° C, the discoloration of the fabric and the fastness to rubbing of the dye will decrease, and if it is much lower than 150 ° C, the productivity will decrease.

  The flame-retardant fabric of the present invention can be suitably used as a transport equipment interior material such as a car seat, a car mat, and a ceiling material.

  EXAMPLES Hereinafter, although an Example and a comparative example are shown and this invention is demonstrated concretely, this invention is not restrict | limited to the following Example.

[Measurement method and evaluation method]
The resin blended in the coating agent and the flame-retardant processed fabric were measured and evaluated by the following methods.

Gel fraction:
(1) The acrylic resin to be measured was coated on a glass plate so that the film thickness after drying was 0.9 to 1.3 mm, left at room temperature for 2 days, and then dried at 150 ° C. for 3 minutes. A sample having a width of 3 cm, a length of 4 cm, and a thickness of 0.9 mm to 1.3 mm was cut from the obtained film to obtain a test piece.
(2) After dipping the test piece in acetone for 24 hours, the insoluble matter was filtered and dried at 65 ° C. for 4 hours. The weight before and after immersion was measured, and the value obtained by the following formula was used as the gel fraction.

Formula 1

Weight residual rate after film burning:
(1) The acrylic resin to be measured was coated on a glass plate so that the film thickness after drying was 0.9 to 1.3 mm, left at room temperature for 2 days, and then dried at 150 ° C. for 3 minutes.
A sample having a width of 3 cm, a length of 8 cm, and a thickness of 0.9 mm to 1.3 mm was cut from the obtained film to obtain a test piece.
(2) The test piece was burned for 30 seconds, and the weight before and after burning was measured. It was assumed that the ones dropped during combustion were gone. The value obtained by the following formula was defined as the weight residual ratio.

Formula 2

Flame retardance:
According to the combustion test of JIS D1201 and ISO 3795.

Wrinkle:
5 ml of water and 95 ° C. warm water were dropped from the front and back of the polyester fabric coated with flame retardant on the back side, and whether or not black or white ring spots were generated after 24 hours was confirmed visually by 10 judges. Grade 4 or higher was accepted.
* Judgment Grade 5: 0 people can see ring juniors 4th grade: 1 people can see ring juniors 3rd grade: 3 people or less can see ring jimi 2nd grade: I see ring jimi 5 people or less, 1st grade: 10 people can see ring jimi

[Example 1]
Cross-linked acrylic resin (gel fraction 88%, weight residual ratio after film combustion 94%, non-volatile content 45%, Rikabond manufactured by Chuo Rika Co., Ltd.), 30 parts alkyl phosphate metal salt (manufactured by Clariant), urethane association type Thickener (Biscon from Shin-Nakamura Chemical Co., Ltd.) (non-volatile content 50%) 5 parts, Tartarbutyl cellosolve (Maruzen Petrochemical Co., Ltd. Swabolbu ETB) 2 parts, Acetylene glycol (non-volatile content 80%, Nissin Chemical Orphine) 0.08 part and 47 parts of water were blended to prepare a coating agent.
The obtained coating agent was applied to the back surface of a polyester fabric having a basis weight of 300 g / m ² and a thickness of 0.8 mm using a knife coater so that the coating amount after drying was 94 g / m ² and dried at 150 ° C. for 3 minutes. Thus, a flame-retardant processed fabric was obtained.
About the obtained fabric, the burning rate and the wrinkle property were measured.

[Example 2]
Cross-linked acrylic resin (gel fraction 88%, weight retention after film combustion 94%, non-volatile content 45%, Rikabond manufactured by Chuo Rika Co., Ltd.) 33 parts, aluminum hydroxide 31 parts, alkyl phosphate metal salt (manufactured by Clariant) 5 parts, urethane associative thickener (non-volatile content: 50%) (biscon from Shin-Nakamura Chemical Co., Ltd.), tertiary butyl cellosolve (Maruzen Petrochemical Co., Ltd., Swatholve ETB), 0.5 part, acetylene glycol (non-volatile content: 80%) 0.03 part of Nissin Chemical Co., Ltd. Olfin) and 29 parts of water were blended to prepare a coating agent.
A coating agent was applied to the back surface of the polyester fabric of the same type as in Example 1 using a knife coater so that the coating amount after drying was 94 g / m ^2, and dried at 150 ° C. for 3 minutes to obtain a flame-retardant processed fabric.
In the same manner as in Example 1, the burning rate and the wrinkling property were measured.

[Example 3]
A coating agent was prepared in the same manner as in Example 2 except that the composition of the coating agent was as shown in Table 1, and a flame-retardant processed fabric was obtained. Similarly, the burning rate and wrinkling properties were measured.

[Comparative Example 1]
Acrylic resin containing no epoxy group and having no self-crosslinkability (gel fraction 75%, residual weight after film combustion 75%, non-volatile content 45%, DIC's Boncoat) 37 parts, aluminum hydroxide 34 parts, urethane 2 parts of an associative thickener (non-volatile content 50%) and 26 parts of water were blended to prepare a coating agent.
A coating agent was applied to the back surface of the same type of polyester fabric as in Example 1 using a knife coater so that the coating amount after drying was 98 g / m ^2, and dried at 150 ° C. for 3 minutes to obtain a flame-retardant processed fabric.
In the same manner as in Example 1, the burning rate and the wrinkling property were measured.

[Comparative Examples 2 to 11]
A coating agent was prepared in the same manner as in Comparative Example 1 except that the composition of the coating agent and the amount applied to the fabric were as shown in Table 1, and a flame-retardant processed fabric was obtained. Similarly, the burning rate and wrinkling properties were measured.
FRX (manufactured by Clariant) was used as ammonium polyphosphate, and bigol (manufactured by Daikyo Chemical Co., Ltd.) was used as the phosphoric ester amide.

  Table 1 shows the measurement results of Examples 1 to 3 and Comparative Examples 1 to 11, the coating amount, the burning rate, and the wrinkling property. Regarding the burning rate, “SE” in the table means self-extinguishing properties.

  As shown in the above table, it can be seen that the flame-retardant processed fabric using the coating agents of Examples 1 to 3 has high flame retardancy and does not cause wrinkles. On the other hand, in the examples in which the cross-linked acrylic resin was not used (Comparative Examples 1 to 6), the burning rate exceeded 100 mm / min or generation of wrinkles was observed. Further, in the case where the flame retardant was only aluminum hydroxide (Comparative Example 7), the burning rate was rejected, the flame retardant which was not an alkyl phosphate metal salt was used, and the compatibility improver was not used (Comparative) In Examples 8 to 11), the wrinkling property and / or the burning rate were not achieved.

[Examples 4 to 6]
Each flame-retardant coating agent which does not contain aluminum hydroxide having the composition shown in Table 2 was obtained.
The obtained coating agent was applied to the back surface of a polyester fabric having a basis weight of 270 g / m ² and a thickness of 0.6 mm using a knife coater and dried at 150 ° C. for 3 minutes to obtain a flame-retardant processed fabric.
About the obtained fabric, the burning rate and the wrinkle property were measured.

[Examples 7 to 12]
Various coating agents containing various compatibility improvers shown in Table 2 were obtained.
The obtained coating agent was applied to the same type of fabric as in Examples 4 to 6 and dried to obtain a flame-retardant processed fabric. In the same manner as in Examples 4 to 6, the burning rate and the wrinkling property were measured.

[Comparative Example 12]
Acrylic resin that does not contain an epoxy group and does not have self-crosslinkability (gel fraction 75%, weight residual ratio after film combustion 75%, non-volatile content 45%, DIC's Boncoat) 35 parts, alkyl phosphate metal salt (Clariant 26 parts), hydroxyethyl cellulose (Clariant Tyroze) 1 part, acetylene glycol (non-volatile content 80%, Nissin Chemical Orphine) 1 part and water 37 parts were blended to prepare a coating agent.
A coating agent was applied to the back surface of the polyester fabric of the same type as in Example 4 using a knife coater so that the coating amount after drying was 59 g / m ^2, and dried at 150 ° C. for 3 minutes to obtain a flame-retardant processed fabric. In the same manner as in Example 4, the burning rate and the wrinkling property were measured.

[Comparative Examples 13 to 21]
A coating agent was prepared in the same manner as in Comparative Example 12 except that the composition of the coating agent and the amount applied to the fabric were as shown in Table 2, and a flame-retardant processed fabric was obtained. Similarly, the burning rate and wrinkling properties were measured.
Heidilite H-32 (manufactured by Showa Denko) as aluminum hydroxide, FRX-304 (manufactured by Clariant) as ammonium polyphosphate, Bigol (manufactured by Daikyo Chemical Co., Ltd.) as phosphoric ester amide, and n-butyl cellosolve ( Sankyo Chemical Co., Ltd., boiling point 171 ° C.), DKS-250 (Daiichi Kogyo Seiyaku Co., Ltd.) was used as the sucrose fatty acid ester, and Amphital 20N (Kao Corporation) was used as the alkylamine oxide.

  Table 2 shows the measurement results of the compositions, coating amounts, burning rates, and wrinkling properties of Examples 4 to 12 and Comparative Examples 12 to 21. Regarding the burning rate, “SE” in the table means self-extinguishing properties.

  As shown in the above table, it can be seen that the flame-retardant processed fabric using the coating agent having the composition of the present invention of Examples 4 to 12 has high flame retardancy and does not cause wrinkles. On the other hand, an example not using a cross-linked acrylic resin (Comparative Example 12), an example not using a low-boiling compatibility improver (Comparative Example 13), an example using a large amount of acetylene glycol (Comparative Example 14), and a boiling point of 150 ° C. Examples using higher compatibility improvers (Comparative Examples 15 to 17) have problems with wrinkling, and examples without using acetylene glycol (Comparative Examples 16 to 21) have problems with wrinkling. There was also an example (Comparative Example 19) in which the flammability was insufficient.

That is, the present invention is difficult to contain a crosslinkable acrylic resin, aluminum trisdiethylphosphinate, aluminum trismethylethylphosphinate or aluminum trisdiphenylphosphinate , urethane associative thickener, acetylene glycol and a compatibility improver as a flame retardant component. Non-volatile component ratio after drying at 150 [deg.] C. is a flame retardant component of 0.3 to 2.0, urethane associative thickener 0.05 To 0.2, acetylene glycol 0.001 to 0.02, and the compatibility improver has a boiling point of 80 to 150 ° C. and is a component that does not remain after drying. It is related with the flame-retardant coating agent characterized by mix | blending in the ratio of 0.01-0.2 with respect to 0.

The present invention further contains aluminum hydroxide, and the aluminum hydroxide has a non-volatile component ratio after drying at 150 ° C. of 0.9 to 2.5 with respect to the cross-linked acrylic resin 1.0. It is related with the said flame-retardant coating agent characterized by being mix | blended.
Aluminum hydroxide is considered to have a function as a flame retardant aid, and when aluminum hydroxide is added, the amount of the flame retardant component used can be reduced, and thus high boiling point dispersion that causes wrinkles The amount of agent used can be reduced, and the occurrence of wrinkles can be further suppressed.

The cross-linked acrylic resin, flame retardant component , urethane associative thickener, and acetylene glycol are non-volatile after the flame retardant coating agent of the present invention is processed into a fabric and subjected to a drying step (for example, about 150 ° C. for about 3 minutes). It is a component remaining in the fabric as a component. The ratio of these non-volatile components is 0.3 to 2.0 for the flame retardant component with respect to the cross-linked acrylic resin 1.0. When the content ratio of the flame retardant component is less than 0.3, the flame retardancy is insufficient, and when the content ratio is more than 2.0, the treated fabric is wrinkled. The urethane associative thickener is contained at a ratio of 0.05 to 0.2 with respect to 1.0 of the cross-linked acrylic resin. If the urethane associative thickener is less than 0.05, the thickening is not sufficient, so that the flame retardant coating agent penetrates to the fabric surface, and if it exceeds 0.2, the viscosity is high and the coatability is poor. Acetylene glycol is contained at a ratio of 0.001 to 0.02 with respect to 1.0 of the cross-linked acrylic resin. When the amount of acetylene glycol is less than 0.001, particularly the flame retardant component cannot be sufficiently dispersed in the coating agent, and when it is more than 0.02, the fabric is wrinkled.

Furthermore, the coating agent of the present invention contains a compatibility improver as a component that does not substantially remain on the fabric after the drying step. The compatibility improver is an organic solvent component having both hydrophilicity and hydrophobicity that has a function of stably dispersing components such as a flame retardant component together with acetylene glycol in the coating agent.
As the compatibility improver, one having a boiling point of 80 to 150 ° C. is used. However, a compatibility improver having a boiling point lower than 80 ° C. volatilizes during transportation and storage, and the quality stability of the coating agent is not sufficient. There is a possibility that the compatibility improver having a boiling point higher than 150 ° C. is not preferable because it is not sufficiently removed in the drying step and causes wrinkles.

[Example 1]
30 parts of cross-linked acrylic resin (gel fraction 88%, weight retention after film combustion 94%, nonvolatile content 45%, Rikabond manufactured by Chuo Rika Co., Ltd.), aluminum trisdiethylphosphinate, aluminum trismethylethylphosphinate or trisdiphenylphosphine 16 parts of aluminum acid (Clariant), 5 parts of urethane associative thickener (Biscon, Shin-Nakamura Chemical Co., Ltd.) (non-volatile content 50%), 2 parts of tert-butyl cellosolve (Suwasolve ETB, Maruzen Petrochemical Co.), acetylene glycol (Non-volatile content 80%, Nissin Chemical Orphine) 0.08 part and 47 parts of water were blended to prepare a coating agent.
The obtained coating agent was applied to the back surface of a polyester fabric having a basis weight of 300 g / m ² and a thickness of 0.8 mm using a knife coater so that the coating amount after drying was 94 g / m ² and dried at 150 ° C. for 3 minutes. Thus, a flame-retardant processed fabric was obtained.
About the obtained fabric, the burning rate and the wrinkle property were measured.

[Example 2]
Cross-linked acrylic resin (gel fraction 88%, weight residual ratio after film combustion 94%, nonvolatile content 45%, Rikabond manufactured by Chuo Rika Co., Ltd.) 33 parts, aluminum hydroxide 31 parts, aluminum trisdiethylphosphinate , trismethylethylphosphine 5 parts of aluminum oxide or aluminum trisdiphenylphosphinate (Clariant), 2 parts of urethane associative thickener (non-volatile content 50%) (Biscon made by Shin-Nakamura Chemical Co., Ltd.), tertiary butyl cellosolve (Suwasolve ETB, Maruzen Petrochemical Co., Ltd.) ) 0.5 part, 0.03 part of acetylene glycol (non-volatile content 80%, Nissin Chemical Orphine) and 29 parts of water were blended to prepare a coating agent.
A coating agent was applied to the back surface of the polyester fabric of the same type as in Example 1 using a knife coater so that the coating amount after drying was 94 g / m ^2, and dried at 150 ° C. for 3 minutes to obtain a flame-retardant processed fabric.
In the same manner as in Example 1, the burning rate and the wrinkling property were measured.

As shown in the above table, it can be seen that the flame-retardant processed fabric using the coating agents of Examples 1 to 3 has high flame retardancy and does not cause wrinkles. On the other hand, in the examples in which the cross-linked acrylic resin was not used (Comparative Examples 1 to 6), the burning rate exceeded 100 mm / min or generation of wrinkles was observed. Moreover, in the example (Comparative Example 7) in which the flame retardant was only aluminum hydroxide, the burning rate was rejected, and a flame retardant that was not aluminum trisdiethylphosphinate, aluminum trismethylethylphosphinate or aluminum trisdiphenylphosphinate was used, And in the example (Comparative Examples 8-11) which did not use a compatibility improvement agent, the wrinkle property and / or the combustion rate were not achieved.

[Comparative Example 12]
Acrylic resin that does not contain an epoxy group and does not have self-crosslinkability (gel fraction 75%, weight residual ratio after film combustion 75%, nonvolatile content 45%, DIC's Boncoat) 35 parts, aluminum trisdiethylphosphinate , tris 26 parts of aluminum methylethylphosphinate or aluminum trisdiphenylphosphinate (manufactured by Clariant), 1 part of hydroxyethylcellulose (Tyroze from Clariant), 1 part of acetylene glycol (80% non-volatile content, Olphine from Nissin Chemical) and water 37 Parts were blended to make a coating agent.
A coating agent was applied to the back surface of the polyester fabric of the same type as in Example 4 using a knife coater so that the coating amount after drying was 59 g / m ^2, and dried at 150 ° C. for 3 minutes to obtain a flame-retardant processed fabric. In the same manner as in Example 4, the burning rate and the wrinkling property were measured.

Claims (6)

A flame retardant coating agent comprising a crosslinkable acrylic resin, an alkyl phosphate metal salt, a urethane associative thickener, acetylene glycol and a compatibility improver,
The non-volatile component ratio after drying at 150 ° C. is 0.3 to 2.0 alkyl phosphate metal salt, 0.05 to 0.2 urethane associative thickener, acetylene with respect to the cross-linked acrylic resin 1.0. Glycol 0.001-0.02,
The compatibility improver has a boiling point of 80 to 150 ° C. and is a component that does not remain after drying, and is blended at a ratio of 0.01 to 0.2 with respect to the nonvolatile component 1.0 of the cross-linked acrylic resin. A flame retardant coating agent characterized by Furthermore, aluminum hydroxide is contained, and the aluminum hydroxide is blended at a ratio of non-volatile components after drying at 150 ° C. of 0.9 to 2.5 with respect to the cross-linked acrylic resin 1.0. The flame retardant coating agent according to claim 1. The flame retardant coating agent according to claim 1 or 2, wherein the cross-linked acrylic resin has a gel fraction and a weight residual ratio after combustion of 80% or more. The compatibility improver is one or more compatibility improvers selected from the group consisting of isopropyl alcohol, normal propyl alcohol, methyl cellosolve, ethyl cellosolve, isopropyl cellosolve and tertiary butyl cellosolve. The flame-retardant coating agent according to any one of claims 1 to 3. The flame-retardant processed fabric processed with the flame-retardant coating agent in any one of Claims 1-4. The flame retardant processed fabric according to claim 5, wherein the flame retardant processed fabric is a fabric having a flame retardant coating only on one side of a polyester fabric having a basis weight of 250 to 400 g / m ² and a thickness of 1.5 mm or less. Processed fabric.