阅读说明：本技术 一种耐高温pvc地板印刷油墨及其制备方法 (High-temperature-resistant PVC floor printing ink and preparation method thereof ) 是由 郭立民 郭智远 张良祥 程荣致 柯耀进 于 2020-12-28 设计创作，主要内容包括：本发明公开了一种耐高温PVC地板印刷油墨及其制备方法,涉及塑胶地板技术领域,旨在解决当地板温度提高至135-140℃时,热压贴合后,产品呈现表面发白等不良现象的问题。其技术方案要点是包括按质量百分数含量计的如下组分,氯醋树脂8-12％、丙烯酸树脂3-5％、主分散剂0.3-0.7％、助分散剂0.3-0.7％、热安定剂1-3％、色粉3-7％、环己酮3-7％、醋酸丁酯10-16％、4-甲基-2-戊酮15-25％、丁酮35-45％,加入热变形温度较高的丙烯酸树脂(Heat Distortion Temp约100℃)后,PVC地板印刷油墨的耐高温热压贴合性能提升；耐热压贴合性提升后,可以加快客户贴合速度(减少贴合时间),提升产能；针对较厚的底膜压贴,一般需要较高温度去贴合,提高油墨耐热压贴合性,可防止高温贴合反白等不良现象的产生。(The invention discloses high-temperature-resistant PVC floor printing ink and a preparation method thereof, relates to the technical field of plastic floors, and aims to solve the problem that when the temperature of a floor is increased to 135-140 ℃, the surface of a product is whitened after hot-pressing and attaching. The technical scheme is characterized by comprising the following components, by mass, 8-12% of vinyl chloride-vinyl acetate copolymer, 3-5% of acrylic resin, 0.3-0.7% of main dispersant, 0.3-0.7% of auxiliary dispersant, 1-3% of thermal stabilizer, 3-7% of toner, 3-7% of cyclohexanone, 10-16% of butyl acetate, 15-25% of 4-methyl-2-pentanone and 35-45% of butanone, wherein after the acrylic resin with high thermal deformation temperature (about 100 ℃ of Heat deformation Temp) is added, the high-temperature and hot-pressing resistance and bonding performance of the PVC floor printing ink is improved; after the hot-pressing resistance is improved, the laminating speed of a client can be increased (the laminating time is reduced), and the productivity is improved; the laminating of a thicker basement membrane generally needs higher temperature to laminate, improves the hot pressing resistance and the laminating property of printing ink, and can prevent the generation of adverse phenomena such as high-temperature laminating whitening and the like.)

1. The high-temperature-resistant PVC floor printing ink is characterized by comprising the following components in parts by weight: comprises the following components in percentage by mass,

2. the printing ink for the high-temperature-resistant PVC floor as claimed in claim 1, wherein: the vinyl chloride-vinyl acetate copolymer resin is fat-soluble binary vinyl chloride-vinyl acetate copolymer resin, and the K value range of the vinyl chloride-vinyl acetate copolymer resin is 58-60.

3. The printing ink for the high-temperature-resistant PVC floor as claimed in claim 1, wherein: the main dispersant is a product of Luborun American company model Luborun (American) hyper-dispersant 24000.

4. The printing ink for the high-temperature-resistant PVC floor as claimed in claim 1, wherein: the dispersion aid is a product of Luborun American type Luborun (American) hyper-dispersant 8200.

5. The printing ink for the high-temperature-resistant PVC floor as claimed in claim 1, wherein: the thermal stabilizer is an organic tin thermal stabilizer.

6. The method for preparing the high temperature resistant PVC floor printing ink according to any one of claims 1 to 5, wherein the method comprises the following steps: comprises the following steps of (a) carrying out,

the method comprises the following steps: weighing the materials, namely weighing the vinyl chloride-vinyl acetate copolymer, the acrylic resin, the main dispersing agent, the auxiliary dispersing agent, the thermal stabilizer, the toner, the cyclohexanone, the butyl acetate, the 4-methyl-2-pentanone and the butanone according to the proportion;

step two: sequentially adding part of butanone, all main dispersing agents, all auxiliary dispersing agents, all toner and part of vinyl chloride-vinyl acetate copolymer into a stirring container, and stirring for 30-90min until all components are uniformly mixed to obtain a mixture;

step three: adding the mixture obtained by stirring in the step two into a grinder, and circularly grinding for 2-3 hours to obtain a ground semi-finished product;

step four: adding the semi-finished product obtained by grinding in the third step into a stirring container, adding the rest butanone, all 4-methyl-2-pentanone, all butyl acetate, all cyclohexanone, all heat stabilizer, the rest chlorine vinegar resin and all acrylic resin, and stirring for 30-100 min;

step five: and filtering and packaging the finished product of the printing ink obtained in the fourth step by using a 200-mesh filter screen.

7. The preparation method of the high-temperature-resistant PVC floor printing ink as claimed in claim 6, wherein the printing ink comprises: in the second step, the stirring speed of the stirring container is more than or equal to 800 rpm.

8. The preparation method of the high-temperature-resistant PVC floor printing ink as claimed in claim 6, wherein the printing ink comprises: the rotating speed of the grinder in the third step is more than or equal to 900 rpm.

9. The preparation method of the high-temperature-resistant PVC floor printing ink as claimed in claim 6, wherein the printing ink comprises: the rotating speed of the stirring container in the fourth step is 800-900 rpm.

Technical Field

The invention relates to the technical field of plastic floors, in particular to high-temperature-resistant PVC floor printing ink and a preparation method thereof.

Background

The plastic floor (PVC floor) mainly comprises a polyvinyl chloride material (PVC). The floor can be made into two types, one type is homogeneous and transparent, namely, the pattern materials from the bottom to the surface are the same; the other is a composite type, namely, the top layer is a pure PVC transparent layer, and a printing layer and a foaming layer are added below the pure PVC transparent layer. The PVC flooring is widely used in various aspects of homes and businesses due to its rich color and variety of colors.

The common hot-pressing bonding temperature of PVC plastic floor in the industry is 125-.

However, when the temperature is increased to 135-140 ℃, the product has the undesirable phenomena of whitening surface after hot pressing and bonding, and thus needs to be further improved.

Disclosure of Invention

The invention aims to provide high-temperature-resistant PVC floor printing ink which has the effect of improving the heat-pressure-resistant laminating performance of a PVC floor.

The technical purpose of the invention is realized by the following technical scheme:

the high-temperature-resistant PVC floor printing ink comprises the following components in percentage by mass,

the invention is further configured to: the vinyl chloride-vinyl acetate copolymer resin is fat-soluble binary vinyl chloride-vinyl acetate copolymer resin, and the K value range of the vinyl chloride-vinyl acetate copolymer resin is 58-60.

The invention is further configured to: the main dispersant is a product of Luborun American company model Luborun (American) hyper-dispersant 24000.

The invention is further configured to: the dispersion aid is a product of Luborun American type Luborun (American) hyper-dispersant 8200.

The invention is further configured to: the thermal stabilizer is an organic tin thermal stabilizer.

The invention also aims to provide a preparation method of the high-temperature-resistant PVC floor printing ink.

In order to achieve the purpose, the application provides the following technical scheme: comprises the following steps of (a) carrying out,

the method comprises the following steps: weighing the materials, namely weighing the vinyl chloride-vinyl acetate copolymer, the acrylic resin, the main dispersing agent, the auxiliary dispersing agent, the thermal stabilizer, the toner, the cyclohexanone, the butyl acetate, the 4-methyl-2-pentanone and the butanone according to the proportion;

step two: sequentially adding part of butanone, all main dispersing agents, all auxiliary dispersing agents, all toner and part of vinyl chloride-vinyl acetate copolymer into a stirring container, and stirring for 30-90min until all components are uniformly mixed to obtain a mixture;

step three: adding the mixture obtained by stirring in the step two into a grinder, and circularly grinding for 2-3 hours to obtain a ground semi-finished product;

step four: adding the semi-finished product obtained by grinding in the third step into a stirring container, adding the rest butanone, all 4-methyl-2-pentanone, all butyl acetate, all cyclohexanone, all heat stabilizer, the rest chlorine vinegar resin and all acrylic resin, and stirring for 30-100 min;

step five: and filtering and packaging the finished product of the printing ink obtained in the fourth step by using a 200-mesh filter screen.

The invention is further configured to: in the second step, the stirring speed of the stirring container is more than or equal to 800 rpm.

The invention is further configured to: the rotating speed of the grinder in the third step is more than or equal to 900 rpm.

The invention is further configured to: the rotating speed of the stirring container in the fourth step is 800-900 rpm.

In conclusion, the beneficial technical effects of the invention are as follows:

after adding acrylic resin (about 100 ℃ C.) with higher thermal deformation temperature, the high-temperature-resistant hot-pressing bonding performance of the PVC floor printing ink is improved;

after the hot-pressing resistance is improved, the laminating speed of a client can be increased (the laminating time is reduced), and the productivity is improved;

the laminating of a thicker basement membrane generally needs higher temperature to laminate, improves the hot pressing resistance and the laminating property of printing ink, and can prevent the generation of adverse phenomena such as high-temperature laminating whitening and the like.

Detailed Description

The following detailed description of the preferred embodiments of the present invention is provided to enable those skilled in the art to more readily understand the advantages and features of the present invention, and to clearly and unequivocally define the scope of the present invention.

It is worth to be noted that the vinyl chloride-vinyl acetate copolymer used in the invention is fat-soluble binary vinyl chloride-vinyl acetate copolymer (vinyl acetate content is 10%), the K value of the vinyl chloride-vinyl acetate copolymer is in the range of 58-60, and domestic or imported resins meeting the above conditions can be used;

the main dispersant is a product of Luborun American company model Luborun (American) hyper-dispersant 24000 and is used for dispersing toner pigments;

the assistant dispersant is a product of Luborun American company model Luborun (American) hyper-dispersant 8200 and is used for assisting in dispersing the toner pigment;

the thermal stabilizer is an organic tin thermal stabilizer, so that the thermal stability of the resin is improved, and the resin is prevented from aging and yellowing due to hot pressing;

the other raw materials are common commercial products, and thus the sources thereof are not particularly limited.

Examples 1 to 5

The contents of the components are shown in the following table according to the mass ratio:

TABLE 1 table of the contents of the components of the PVC floor printing inks of examples 1 to 5

Components	Example 1	Example 2	Example 3	Example 4	Example 5
						Vinyl chloride-vinyl acetate copolymer	8kg	10kg	12kg	8kg	12kg
Acrylic resin	5kg	4kg	3kg	5kg	3kg
						Main dispersing agent	0.3kg	0.5kg	0.7kg	0.3kg	0.7kg
Dispersing aid	0.7kg	0.5kg	0.3kg	0.7kg	0.3kg
						Heat stabilizer	3kg	2kg	1kg	2kg	2kg
Toner powder	3kg	5kg	7kg	4kg	6kg
						Cyclohexanone	7kg	5kg	3kg	7kg	3kg
Acetic acid butyl ester	10kg	13kg	16kg	13kg	11kg
						4-methyl-2-pentanone	25kg	20kg	15kg	25kg	17kg
Butanone	38kg	40kg	42kg	35kg	45kg

Example 6

Based on example 1, the preparation of example 1 was as follows,

the method comprises the following steps: weighing 8kg of vinyl chloride-vinyl acetate copolymer, 5kg of acrylic resin, 0.3kg of main dispersant, 0.7kg of auxiliary dispersant, 3kg of thermal stabilizer, 3kg of toner, 7kg of cyclohexanone, 10kg of butyl acetate, 25kg of 4-methyl-2-pentanone and 38kg of butanone according to the proportion;

step two: sequentially adding 28.5kg of partial butanone, all main dispersing agents, all auxiliary dispersing agents, all toner and 2.4kg of partial vinyl chloride-vinyl acetate copolymer into a stirring container, and stirring at the rotating speed of 1000rpm for 30min until all components are uniformly mixed to obtain a mixture;

step three: adding the mixture obtained by stirring in the step two into a grinder, and circularly grinding for 2 hours at the rotating speed of 1000rpm to obtain a ground semi-finished product;

step four: adding the semi-finished product obtained by grinding in the third step into a stirring container, adding 9.5kg of residual butanone, all 4-methyl-2-pentanone, all butyl acetate, all cyclohexanone, all thermal stabilizer, 5.6kg of residual chlorine vinegar resin and all acrylic resin, and stirring for 30min at the rotating speed of 900 rpm;

step five: and filtering and packaging the finished product of the printing ink obtained in the fourth step by using a 200-mesh filter screen.

Example 7

Based on example 2, the preparation method of example 2 is as follows,

the method comprises the following steps: weighing 10kg of vinyl chloride-vinyl acetate copolymer, 4kg of acrylic resin, 0.5kg of main dispersant, 0.5kg of auxiliary dispersant, 2kg of thermal stabilizer, 5kg of toner, 5kg of cyclohexanone, 13kg of butyl acetate, 20kg of 4-methyl-2-pentanone and 40kg of butanone according to the proportion;

step two: sequentially adding 30kg of part of butanone, all main dispersing agents, all auxiliary dispersing agents, all toner and 3kg of part of vinyl chloride-vinyl acetate copolymer into a stirring container, and stirring at the rotating speed of 900rpm for 60min until all components are uniformly mixed to obtain a mixture;

step three: adding the mixture obtained by stirring in the step two into a grinder, and circularly grinding for 2.5 hours at the rotating speed of 950rpm to obtain a ground semi-finished product;

step four: adding the semi-finished product obtained by grinding in the third step into a stirring container, adding 10kg of residual butanone, all 4-methyl-2-pentanone, all butyl acetate, all cyclohexanone, all thermal stabilizer, 7kg of residual chlorine vinegar resin and all acrylic resin, and stirring for 70min at the rotating speed of 850 rpm;

step five: and filtering and packaging the finished product of the printing ink obtained in the fourth step by using a 200-mesh filter screen.

Example 8

Based on example 3, the preparation of example 3 was as follows,

the method comprises the following steps: weighing 12kg of vinyl chloride-vinyl acetate copolymer, 3kg of acrylic resin, 0.7kg of main dispersant, 0.3kg of auxiliary dispersant, 1kg of thermal stabilizer, 7kg of toner, 3kg of cyclohexanone, 16kg of butyl acetate, 15kg of 4-methyl-2-pentanone and 42kg of butanone according to the proportion;

step two: adding 31.5kg of part of butanone, all main dispersing agents, all auxiliary dispersing agents, all toner and 3.6kg of part of vinyl chloride-vinyl acetate copolymer into a stirring container in sequence, and stirring for 90min at the rotating speed of 800rpm until all components are uniformly mixed to obtain a mixture;

step three: adding the mixture obtained by stirring in the step two into a grinder, and circularly grinding for 3 hours at the rotating speed of 900rpm to obtain a ground semi-finished product;

step four: adding the semi-finished product obtained by grinding in the third step into a stirring container, adding 10.5kg of residual butanone, all 4-methyl-2-pentanone, all butyl acetate, all cyclohexanone, all thermal stabilizer, 8.4kg of residual chlorine vinegar resin and all acrylic resin, and stirring for 100min at the rotating speed of 800 rpm;

step five: and filtering and packaging the finished product of the printing ink obtained in the fourth step by using a 200-mesh filter screen.

Example 9

Based on example 4, the preparation of example 4 was as follows,

the method comprises the following steps: weighing 8kg of vinyl chloride-vinyl acetate copolymer, 5kg of acrylic resin, 0.3kg of main dispersant, 0.7kg of auxiliary dispersant, 2kg of thermal stabilizer, 4kg of toner, 7kg of cyclohexanone, 13kg of butyl acetate, 25kg of 4-methyl-2-pentanone and 35kg of butanone according to the proportion;

step two: sequentially adding 26kg of partial butanone, all main dispersing agents, all auxiliary dispersing agents, all toner and 2.4kg of partial vinyl chloride-vinyl acetate copolymer into a stirring container, and stirring at 870rpm for 70min until all components are uniformly mixed to obtain a mixture;

step three: adding the mixture obtained by stirring in the step two into a grinder, and circularly grinding for 2.4 hours at the rotating speed of 930rpm to obtain a ground semi-finished product;

step four: adding the semi-finished product obtained by grinding in the third step into a stirring container, adding the rest 9kg of butanone, all 4-methyl-2-pentanone, all butyl acetate, all cyclohexanone, all heat stabilizer, all 5.6kg of chlorine vinegar resin and all acrylic resin, and stirring for 60min at the rotating speed of 860 rpm;

step five: and filtering and packaging the finished product of the printing ink obtained in the fourth step by using a 200-mesh filter screen.

Example 10

Based on example 5, the preparation of example 5 was as follows,

the method comprises the following steps: weighing 12kg of vinyl chloride-vinyl acetate copolymer, 3kg of acrylic resin, 0.7kg of main dispersant, 0.3kg of auxiliary dispersant, 2kg of thermal stabilizer, 6kg of toner, 3kg of cyclohexanone, 11kg of butyl acetate, 17kg of 4-methyl-2-pentanone and 45kg of butanone according to the proportion;

step two: adding 33kg of part of butanone, all main dispersing agents, all auxiliary dispersing agents, all toner and 3.6kg of part of vinyl chloride-vinyl acetate copolymer into a stirring container in sequence, and stirring at the rotating speed of 950rpm for 80min until all components are uniformly mixed to obtain a mixture;

step three: adding the mixture obtained by stirring in the step two into a grinder, and circularly grinding for 2.5 hours at the rotating speed of 950rpm to obtain a ground semi-finished product;

step four: adding the semi-finished product obtained by grinding in the third step into a stirring container, adding 12kg of residual butanone, all 4-methyl-2-pentanone, all butyl acetate, all cyclohexanone, all thermal stabilizer, 8.4kg of residual chlorine vinegar resin and all acrylic resin, and stirring for 90min at the rotating speed of 900 rpm;

step five: and filtering and packaging the finished product of the printing ink obtained in the fourth step by using a 200-mesh filter screen.

Test 1: the PVC floor printing inks obtained in examples 6 to 10 and the commercially available standard grade inks were tested for adhesion in accordance with the scratch test for paint films of GBT9286-1988 paints and varnishes.

The test method comprises the following steps: the inks of examples 6 to 10, which are commercially available and of a common grade, were printed on PVC material, the print was left for more than 2 hours until the printed film was dry, and 10 × 10 squares of 100 were drawn with a hundred-grid knife, and the cut was made to see the substrate but not just the paint. After the tape is scratched by a hundred-grid knife, the tape does not fall off when tested by an adhesive tape. Firstly, the adhesive tape is stuck to a grid position, the adhesive tape is tightly stuck by pressing down with fingers, then the adhesive tape is torn up by instant force, whether the coating falls off or not is visually observed, and the percentage of the area without falling off in the total area is counted. The Tape model was 3M Transparent Tape 600.

The test results are shown in the following table.

TABLE 2 Baige test results

As shown in Table 2, no peeling phenomenon occurred on the surfaces of the products in examples 6-10 by the Baige test, and it can be seen that the surfaces of the floor printing inks added with the acrylic resin still have excellent adhesion.

Test 2: the PVC floor printing inks obtained in examples 6 to 10 were subjected to a joint strength test with a commercially available general-grade ink.

The method for testing the bonding strength comprises the following steps: (1) coating the printing ink on a PVC material by using an RDS #6 scraper bar;

(2) laminating by using a laminating machine at the laminating temperature (135 ℃ of the upper plate and 130 ℃ of the lower plate) under the laminating pressure of 80KG for 5 minutes; attaching the two sections of pressure for 5 minutes at 100 KG;

(3) cutting the test piece into pieces with the width of 5CM, the length of 15CM and the unit of tensile force N/5 CM;

(4) and testing the peel strength by using a tensile machine, and determining the product as a qualified product when the strength is greater than 10N/5 CM.

The test results are shown in the following table.

TABLE 3 bonding Strength test results

Group of	Bonding Strength (N/5CM)
		Example 6	＞10
Example 7	＞10
		Example 8	＞10
Example 9	＞10
		Example 10	＞10
Commercial regular grade ink	＞10

As shown in Table 3, the bonding strength of the products of examples 6-10 was > 10N/5CM, and it can be seen that the floor printing ink containing acrylic resin still has a high bonding strength on the surface.

Test 3: the PVC floor printing inks obtained in examples 6 to 10 and commercially available general-grade inks were subjected to a hot press discoloration test at 125 ℃ and 130 ℃ and at 135 ℃ and at 140 ℃ respectively.

The test results are shown in table 4.

TABLE 4 statistical results of thermochromism at different temperatures for each group

Group of	125℃	130℃	135℃	140℃
					Example 6	Does not change color	Does not change color	Does not change color	Does not change color
Example 7	Does not change color	Does not change color	Does not change color	Does not change color
					Example 8	Does not change color	Does not change color	Does not change color	Does not change color
Example 9	Does not change color	Does not change color	Does not change color	Does not change color
					Example 10	Does not change color	Does not change color	Does not change color	Does not change color
Commercial regular grade ink	Does not change color	Does not change color	Color change and white reflection	Color change and white reflection

As can be seen from the above table, the hot pressing temperature of the commercially available common grade ink is 125-; when the temperature is increased (135 ℃ C. and 140 ℃ C.), the PVC floor printing ink prepared in the examples 6-10 does not change color and has excellent high-temperature-resistant hot-pressing laminating performance.

The thermal deformation temperature of the vinyl chloride-vinyl acetate resin or polyvinyl chloride resin is generally 70 ℃, and after the acrylic resin (about 100 ℃ in Heat deformation Temp) with higher thermal deformation temperature is added, the high-temperature Heat-resistant and hot-pressing bonding performance of the PVC floor printing ink is improved.

Acrylic resin with good heat resistance is used in the formula, so that the overall heat-pressure-resistant lamination performance of the printing ink for the PVC floor is improved;

after the hot-pressing resistance is improved, the laminating speed of a client can be increased (the laminating time is reduced), and the productivity is improved;

the laminating of a thicker basement membrane generally needs higher temperature to laminate, improves the hot pressing resistance and the laminating property of printing ink, and can prevent the generation of adverse phenomena such as high-temperature laminating whitening and the like.

The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes performed by the present invention or directly or indirectly applied to other related technical fields are included in the scope of the present invention.