JP3521489B2 - Adhesive base for polyacrylic acid cataplasm and production method thereof - Google Patents

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a pressure-sensitive adhesive base for a poultice, which is used by containing a drug and directly applying it to the skin.
More specifically, it relates to a pressure-sensitive adhesive base for a polyacrylic acid-based poultice having excellent initial adhesive strength, stability over time, and shapeability, and a method for producing the same.

[0002]

2. Description of the Related Art Polyacrylic acid and polyacrylic acid salts are used as an adhesive base for a polyacrylic acid type poultice. For example, JP-A-3-161436, JP-A-5
As described in JP-A-9-11061, JP-A-62-63512, and JP-A-61-260014, a polyacrylic acid monovalent salt is used as an essential component and dispersed in a polyhydric alcohol. An acrylic acid aqueous solution is added, or water and polyacrylic acid powder are added to prepare an adhesive base for poultices. However, these conventional techniques have problems in any of important properties as a poultice, such as safety, initial adhesive strength, stability of adhesive strength with time, and shapeability after application to the skin. For example, acrylic acid monomer remains, initial adhesive strength is too low to stick to the skin, those with improved initial adhesive strength are conversely softened by body temperature and remain on the skin after peeling, Further, there is a problem that the adhesive force is deteriorated with time due to the removal of water and the progress of the crosslinking reaction.

In order to solve these problems, Japanese Unexamined Patent Publication No. 6-
In No. 135828, a solid or powdery polyacrylic acid which can be an aqueous solution having a specific viscosity is used together with other water-soluble polymer, so that it is excellent in safety and has a relatively good adhesive property. Techniques for providing agents are disclosed. However, the stability over time and the initial adhesive strength are still insufficient, and since exudation from the non-woven fabric substrate is likely to occur, an adhesive base for poultices having better adhesive properties has been demanded. .

[0004]

Therefore, in the present invention, the initial adhesive strength, the stability of the adhesive strength over time, and the shapeability are all excellent.
Moreover, it is an object of the present invention to provide a high-performance adhesive base for a poultice that does not exude from a nonwoven fabric.

[0005]

The adhesive base for a polyacrylic acid-based poultice according to the present invention has the gist of satisfying all the following adhesive properties. (1) After applying 10 g of an adhesive base to a 14 cm × 10 cm non-woven fabric, a test piece having a length of 10 cm × a width of 5 cm was cut out, left standing at 40 ° C. and 75% RH for 1 day, and then JIS Z
The ball tack value BT ₁ at an inclination angle of 30 ° when the test was carried out according to the tack test method of 0237 is the ball number 2
It is 0 or more. (2) After applying 10 g of the adhesive base to a non-woven fabric of 14 cm × 10 cm, a test piece of 10 cm in length × 5 cm in width is cut out, left standing at 40 ° C. and 75% RH for 15 days, and then JIS Z
Inclination angle of 30 according to the tack test method of 0237
The ball tack value BT _{2 in} degrees is the ball number 13 or more. (3) The above BT ₁ -BT ₂ is 8 or less. (4) 10 g of adhesive base was applied to a non-woven fabric of 14 cm × 10 cm, left still at 40 ° C. and 75% RH for 1 day, and 15
After left standing for a day, it is attached to a stainless steel plate of SUS304.
37 ° C, 60% RH with a load of 10 g / cm ² applied
When left for 6 hours and peeled off, the weight of the adhesive base remaining on the stainless steel plate is less than 0.2 g in all cases.

The above-mentioned adhesive base of the present invention is a solid polyacrylic acid having a weight average molecular weight of 1 × 10 ⁶ or more and / or a neutralization rate of 30 mol% or less (not including 0%, The same) solid polyacrylic acid salt dispersed or dissolved, and polyacrylic acid monovalent salt dispersed or dissolved in a polyhydric alcohol, mixed with water containing a polyvalent metal compound. Preferably there is. Moreover, the solid polyacrylic acid and / or the neutralization rate 3 satisfying the viscosity of a 10% aqueous solution of 1500 cps or more, not the parameter of the weight average molecular weight of 1 × 10 ⁶ or more.
You may use 0 mol% or less of polyacrylic acid salts, and all are a preferable embodiment in order to achieve the adhesive property prescribed | regulated by this invention. Further, the use of a polyhydric alcohol having a C number> OH number ≧ 2 and a linear polyacrylic acid and / or a polyacrylic acid salt having a neutralization ratio of 30 mol% or less also makes it possible to obtain the above high-performance adhesive. It is a preferred embodiment for expressing the property.

The production method for obtaining the pressure-sensitive adhesive base of the present invention is a solid polyacrylic acid having a weight average molecular weight of 1 × 10 ⁶ or more in a polyhydric alcohol and / or a solid polyacrylic acid having a neutralization ratio of 30 mol% or less. Characterized by mixing an acrylic acid salt dispersed or dissolved and a polyacrylic acid monovalent salt dispersed or dissolved in a polyhydric alcohol in the presence of water containing a polyvalent metal compound. . At this time,
Solid polyacrylic acid and / or neutralization rate 30 mol%
The viscosity of the following polyacrylic acid salt in a 10% aqueous solution may be 1500 cps or more. C number>
It is a preferred embodiment of the present invention to use a polyhydric alcohol having an OH number of ≧ 2 and a linear polyacrylic acid and / or a polyacrylic acid salt having a neutralization rate of 30% or less.

[0008]

The present inventors have attempted to increase the molecular weight of polyacrylic acid (salt), and have conducted diligent research by paying attention to the mixing procedure of various raw materials. As a result, when using high-molecular weight polyacrylic acid (salt), an aqueous solution is obtained. It has been found that the adhesive property is remarkably improved when used in a state of being dispersed in a polyhydric alcohol rather than being mixed in the state, and the present invention can be reached. Hereinafter, the present invention will be described in detail.

First, the adhesive base for poultices of the present invention must satisfy the following adhesive properties. (1) After applying 10 g of an adhesive base to a 10 cm × 14 cm non-woven fabric, a test piece having a length of 10 cm × a width of 5 cm is cut out, left standing at 40 ° C. and 75% RH for 1 day, and then JIS Z
The ball tack value BT ₁ at an inclination angle of 30 ° when the test was carried out according to the tack test method of 0237 is the ball number 2
It is 0 or more.

Specifically, after applying 10 g of an adhesive base prepared as a poultice as a raw material as described below to a non-woven fabric,
For example, cover with polyethylene film etc. for surface protection,
Let stand at 40 ° C and 75% RH for one day. 10 cm x 5 cm
The test piece cut out was attached to a ball rolling device shown in JIS Z 0237 with the adhesive base surface facing upward, and the inclination angle was 3
Set at 0 degrees, and from the position 10 cm from the top of the test piece, 1
/ 32 to 31/32 inch stainless steel ball with initial velocity 0
The measured value is defined as a ball number, which is 32 times the diameter of the maximum diameter ball that rolls for 1 minute and stops on the adhesive base. The measurement atmosphere is 25 ° C, 65%
RH.

In the present invention, the ball tack value BT at this time is
₁ was used as a standard for the initial adhesive strength, and BT ₁ of 20 or more was an essential requirement. Considering that the adhesive force decreases because the crosslinking reaction slightly progresses during storage, BT ₁ is 2
When it is less than 0, the initial adhesive strength is low, and thus it is not preferable because it may not be easily attached to the skin and may be peeled off immediately or the joint movement cannot be followed. More preferable BT ₁ is 25 or more.

(2) Add 10 g of the adhesive base to 10 cm × 14 c
After being applied to a non-woven fabric of m, a test piece having a length of 10 cm and a width of 5 cm is cut out and left still at 40 ° C. and 75% RH for 15 days.
The ball tack value BT ₂ at a tilt angle of 30 degrees when the method is performed according to the JIS Z 0237 tack test method is a ball number of 13 or more.

The ball tack value is measured by the method described in BT ₁ above.
Is the same as when measuring. However, BT ₂ is the ball tack value after standing for 15 days after preparing the adhesive base.
With the adhesive base for poultices, it is unavoidable that the adhesive force will decrease because the crosslinking reaction slightly progresses during storage, but in the present invention, the ball tack value BT ₂ after 15 days is 13 as a measure of the change over time. It was decided as above. When BT ₂ is less than 13, adhesive failure occurs when the period from the production of the poultice to the actual delivery to the user is long, which is not preferable. More preferable BT ₂ is 18 or more.

(3) The above BT ₁ -BT ₂ is 8 or less.
As described above, the daily change of the ball tack value is an unavoidable phenomenon, but if BT ₁ -BT ₂ is 8 or less, it can be said that the storage stability is good. When BT ₁ -BT ₂ exceeds 8, the degree of decrease in adhesive strength is too large, which is not preferable.

(4) Add 10 g of adhesive base to 10 cm × 14 c
It is applied to a non-woven fabric of m, and is left still at 40 ° C. and 75% RH for 1 day and after left for 15 days, and then attached to a stainless steel plate of SUS304. 37 with a load of 10 g / cm ² applied
The weight of the pressure-sensitive adhesive base remaining on the stainless steel plate was less than 0.2 g when peeled after being left still at 60 ° C. and 60% RH for 6 hours.

The above requirement (4) defines the shape-forming property and its change over time. A poultice with poor shaping properties may cause "paste residue" when applied to the skin or "drip" in the summer when the room temperature is high. In the present invention, the above-mentioned evaluation test having a good correlation with the adhesiveness to the skin was used as the index of the shapeability. 1 day after preparation of adhesive base, or 15
It cannot be said that the shapeability is good unless the residual adhesion amount after day is less than 0.2 g.

The adhesive base for poultice of the present invention must satisfy all the requirements (1) to (4) of the above adhesive properties.
This is because if even one of these requirements cannot be satisfied, the high-performance pressure-sensitive adhesive base aimed at by the present invention cannot be obtained. Next, the raw material and the manufacturing method of the adhesive base for poultice of the present invention will be described.

The basic raw material of the adhesive base for poultice of the present invention is solid polyacrylic acid and / or a neutralization rate of 30%.
The following polyacrylic acid salts, polyhydric alcohols, polyacrylic acid monovalent salts, water, and polyvalent metal compounds as crosslinking agents.

The solid polyacrylic acid preferably has a weight average molecular weight of 1 × 10 ⁶ or more from the viewpoint of adhesive properties. If it is less than 1 × 10 ⁶ , the initial tackiness decreases and the shapeability also deteriorates. As the viscosity of the solid polyacrylic acid, it is preferable that the viscosity of a 10% aqueous solution is 1500 cps or more. This is because if the viscosity is too low, not only the viscosity when the adhesive base is prepared becomes insufficient, but also the exudation from the nonwoven fabric occurs. The viscosity here is a value measured at 25 ° C. with a Brookfield rotational viscometer.

The solid polyacrylic acid of the present invention is preferably a non-crosslinked linear type. This is because the use of a cross-linked polyacrylic acid does not produce favorable adhesive properties. The method for producing solid polyacrylic acid is not particularly limited, but a known method of drying and pulverizing after polymerization in an aqueous solution is recommended. Specifically, 10-40%
Persulfate, redox,
A known initiator such as azo is added, and at room temperature to 100 ° C,
Polymerization is performed for 1 to 10 hours, and the resulting polyacrylic acid aqueous solution may be dried and then pulverized. Alternatively, aqueous solution static polymerization, reverse phase suspension polymerization, or reverse phase emulsion polymerization may be used.

In the present invention, together with solid polyacrylic acid,
Alternatively, a polyacrylic acid salt having a weight average molecular weight of 1 × 10 ⁶ or more and a neutralization ratio of 30 mol% or less (not including 0%) may be used. If the neutralization rate exceeds 30 mol%, the tackiness and shapeability will be reduced. A more preferable upper limit of the neutralization rate is 10 mol%. When using polyacrylic acid salt, 1
It is preferable to use a 0% aqueous solution having a viscosity of 1500 cps or more. In order to obtain a polyacrylic acid salt having a neutralization rate of 30 mol% or less, a method of performing the above-mentioned aqueous solution polymerization or aqueous solution static thermal polymerization using an acrylic acid salt partially neutralized in advance, or polyacrylic acid It is also possible to employ a method of neutralizing a part. Examples of the alkali used for neutralization include alkali metal such as sodium and potassium and hydroxides of other monovalent metals, ammonia, and water-soluble compounds containing organic amine.

The polyacrylic acid and / or the polyacrylic acid salt having a neutralization rate of 30 mol% or less is first mixed in a solid state with a polyhydric alcohol described below to be in a dispersed or dissolved state. From the viewpoint of dispersion and solubility and the ease of handling,
It is preferable to use powder or flakes. In the present invention, a process of dispersing or dissolving polyacrylic acid and / or a polyacrylic acid salt having a neutralization ratio of 30 mol% or less with another polyacrylic acid monovalent salt, which is another main raw material, or a polyvalent metal compound of a crosslinking agent. In, the use in the state of aqueous solution (including the state where polyhydric alcohol and water are mixed) must be avoided. This is because if the dispersion or the dissolution is performed in an aqueous solution state, it is difficult to obtain the excellent adhesive property that is the object of the present invention. The reason for this is presumed as follows.

That is, when polyacrylic acid or a polyacrylic acid salt having a neutralization rate of 30 mol% or less is dispersed or dissolved in a polyhydric alcohol in advance, the polyhydric alcohol becomes polyacrylic acid (or its neutralization rate of 30%). A carboxyl group derived from polyacrylic acid or a polyacrylic acid salt having a neutralization rate of 30 mol% or less in order to form a protective film by associating around the carboxylic acid portion of (mol% or less of salt) to form a protective colloidal action. Is less likely to undergo a salt exchange reaction with a monovalent polyacrylic acid salt or a cross-linking reaction with a polyvalent metal when a polyvalent metal compound is added. Due to this action, polyacrylic acid or a polyacrylic acid salt having a neutralization ratio of 30 mol% or less exists in the adhesive base material while maintaining a high carboxylic acid density, and therefore, it is considered that excellent adhesive properties can be obtained. .

On the other hand, when the polyacrylic acid in the aqueous solution state is mixed with the monovalent polyacrylic acid salt as in the conventional method, the protective colloid effect by the polyhydric alcohol does not appear, and the salt exchange reaction or the cross-linking reaction is eventually caused. It is easy to occur. For this reason, polyacrylic acid and polyacrylic acid monovalent salt become evenly partially neutralized polyacrylic acid salts, and further a crosslinking reaction by polyvalent metal occurs. Therefore, it is considered difficult to improve all adhesive properties.

The polyhydric alcohol used in the present invention is not particularly limited as long as it can disperse or dissolve polyacrylic acid (or a salt having a neutralization ratio of 30 mol% or less). Specific examples include glycerin, diglycerin, diethylene glycol, polyethylene glycol, propylene glycol, dipropylene glycol, polypropylene glycol, 1,3- or 1,4-butylene glycol, ethylene-propylene glycol copolymer, sorbitol and the like. , Or may be used as a mixture of two or more kinds. In particular, the C number and OH number (hydroxyl group number) of the polyhydric alcohol are C> OH ≧
A slightly hydrophobic polyhydric alcohol such as 2 is preferable because the protective colloid-forming ability is amplified. These polyhydric alcohols are used at least 2 times (weight), preferably 5 times or more, with respect to polyacrylic acid (or a salt having a neutralization ratio of 30 mol% or less). The upper limit of the amount used is 30 times.

The polyacrylic acid monovalent salt used in the present invention is a polyacrylic acid salt which is neutralized in an amount of 40 to 100 mol%, and is clearly different from the above-mentioned polyacrylic acid salt having a neutralization ratio of 30 mol% or less. To be distinguished. Alkali metal salts such as sodium and potassium, other monovalent metal salts, salts such as ammonia and organic amine salts can be used. Also in the polyacrylic acid monovalent salt, those having a polymerization average molecular weight of 1 × 10 ⁶ or more are preferable as in the case of the polyacrylic acid. Even in the monovalent polyacrylic acid salt, the amount is 2 times or more, preferably 5 times or more 3.
It is recommended to contact with water containing a polyvalent metal compound described below in a state of being dispersed or dissolved in a polyhydric alcohol of 0 times or less.

In the adhesive base for poultice of the present invention, a polyvalent metal compound is used as a crosslinking agent. Of these, water-soluble aluminum salts are preferable because they have a high crosslinking rate and excellent shapeability. Specific examples include aluminum hydroxide, aluminum chloride, calcium hydroxide, calcium chloride, aluminum sulfate, ammonium aluminum sulfate, potassium aluminum sulfate, magnesium aluminometasilicate, and dihydroxyaluminum aminoacetate. Among them, aluminum chloride (AlCl ₃・ 6H ₂
O), aluminum acetate, aluminum sulfate, potassium aluminum sulfate, ammonium aluminum sulfate and the like are preferably used.

These water-soluble aluminum salts and other polyvalent metal compounds are polyhydric alcohol dispersions or solutions of the above-mentioned polyacrylic acid and / or salts having a neutralization rate of 30 mol% or less in the state of an aqueous solution or water dispersion. And a polyacrylic acid monohydric salt polyhydric alcohol dispersion or solution.
0.5 to 5% by weight of polyacrylic acid and / or polyacrylic acid having a neutralization rate of 30 mol% or less in the entire adhesive base;
It is preferable to mix the polyacrylic acid monovalent salt in an amount of 0.5 to 5% by weight and the polyvalent metal compound in an amount of 0.05 to 1% by weight.

If necessary, an inorganic filler is added to the adhesive base for poultice of the present invention. As an inorganic filler,
Examples include kaolin, talc, calcium carbonate, mica, titanium oxide, etc., 1 to 20% by weight in the adhesive base for poultices.
Be compounded.

As physiologically active substances, l-menthol, camphor, methyl salicylate, thymol, peppermint oil, diphenhydramine hydrochloride, capsicum extract, chloropheniramine maleate, indomethacin, felbinac, ketoprofen, flurbiprofen, etc. are appropriately added. be able to. When using a lipophilic physiologically active substance, it is preferable to use a known surfactant or solubilizer.

As a specific method for producing the adhesive base for poultice of the present invention, for example, powdery polyacrylic acid and / or polyacrylic acid salt having a neutralization ratio of 30 mol% or less is used at room temperature to 60 ° C. What was added to polyhydric alcohol and well stirred and dispersed or dissolved (Liquid A), and polyacrylic acid monovalent salt were added to polyhydric alcohol at room temperature to 60 ° C, and well stirred to be dispersed or dissolved. (Solution B) are separately produced, and the solution (solution A) and solution (solution B) are used as a polyvalent metal compound aqueous solution or dispersion (solution C) containing a filler or a physiologically active substance as required. A method of mixing well at the same time or gradually is mentioned.

At this time, (solution A) and (solution B) are (C
Do not use it as an aqueous solution until it comes into contact with the liquid. This is because the protective colloid effect due to the association of the polyhydric alcohol is sufficiently exhibited as described above.

The adhesive base for poultices is, for example, non-woven fabric,
Direct coating on a support such as paper or film, or
A poultice can be obtained by a method such as coating on a base material that has been subjected to a peeling treatment and spreading it on these supports.

[0034]

The present invention will be described in more detail with reference to the following examples, but the following examples do not limit the present invention.
All modifications and implementations that do not depart from the spirit of the description below are included in the technical scope of the present invention.

Polymerization Example 1 A separable flask having a capacity of 2 liters equipped with a stirrer, a thermometer, a nitrogen introducing tube and a reflux condenser was charged with 840 g of water and 150 g of acrylic acid and heated to 60 ° C. while blowing nitrogen gas. did. 10% by weight of 2, while stirring
Polymerization was initiated by adding 10 g of a 2'-azobis-2-amidinopropane dihydrochloride aqueous solution. Polymerization was completed after 3 hours to obtain a polyacrylic acid aqueous solution having a solid content of 15% by weight.
This aqueous solution was applied on a Teflon sheet to a thickness of 3 mm, dried with a hot air dryer at 120 ° C. for 2 hours, and the dried product was pulverized to obtain a polymer 1.

Polymerization Example 2 In the same manner as Polymerization Example 1, a polyacrylic acid aqueous solution having a solid content of 15% by weight was obtained. The neutralization rate is 20 in 100 g of this aqueous solution.
%, So that 3% of 5% by weight sodium hydroxide
Was added and mixed uniformly. The obtained aqueous solution was dried and pulverized in the same manner as in Polymerization Example 1 to obtain a polymer 2.

Polymerization Example 3 Polymer 3 was obtained in the same manner as in Polymerization Example 2, except that 66.6 g of 5 wt% sodium hydroxide was added so that the neutralization rate was 40%. Polymerization Example 4 Polymer 4 was obtained in the same manner as in Polymerization Example 2, except that 166.4 g of 5 wt% sodium hydroxide was added so that the neutralization rate was 100%. Polymerization Example 5 In the same manner as in Polymerization Example 1, an aqueous polyacrylic acid solution having a solid content of 15% by weight was obtained. This was directly used as Polymer 5.

Polymerization Example 6 A separable flask having a capacity of 5 liters equipped with a stirrer, a thermometer, a nitrogen introducing tube and a reflux condenser was charged with 1124 g of water and heated to 100 ° C. 140 g of 1% by weight 2,2'-azobis-2-amidinopropane dihydrochloride aqueous solution under atmospheric pressure while blowing nitrogen gas at around the boiling temperature.
2666 g of 0 wt% acrylic acid aqueous solution was added dropwise over 60 minutes with stirring to carry out a polymerization reaction. Then
70 g of a 1% by weight aqueous 2,2′-azobis-2-amidinopropane dihydrochloride solution was added dropwise over 60 minutes, and the mixture was stirred at the boiling temperature of the system for another 30 minutes to complete the polymerization reaction. The obtained polyacrylic acid aqueous solution having a solid content of 20% by weight was applied on a Teflon sheet to a thickness of 3 mm, and 120
Polymer 2 was dried with a hot air dryer at ℃ for 2 hours, and the dried product was pulverized to obtain polymer 6.

The weight average molecular weight of each polymer was measured by GPC. The column is Showa Denko's ion pak K
S-806 was detected by RI using 0.1 molar aqueous phosphoric acid solution (pH 7) as an eluent. As the standard substance, Sowa Kagaku sodium polyacrylate was used. Also, 5
% Viscosity in water (cps) was measured at 25 ° C. with a Brookfield viscometer. The results of measurement of viscosity and molecular weight are shown in Table 1.

[0040]

[Table 1]

Example 1 4.3 parts by weight of the above polymer 1, propylene glycol 6
Part by weight and 20 parts by weight of glycerin were mixed and dispersed to prepare a liquid A. Further, the polymer 4 was mixed and dispersed in 3.7 parts by weight, 6 parts by weight of propylene glycol and 20 parts by weight of glycerin to prepare a liquid B. Furthermore, in 33.7 parts by weight of water, aluminum chloride hexahydrate (AlCl ₃ .6H ₂
O) 0.3 part by weight and kaolin 6 parts by weight were added to prepare a liquid C. Solution A, solution B and solution C were mixed simultaneously and kneaded for 15 minutes. 10 g of the obtained adhesive base is 10 cm × 14 c
Thin non-woven fabric was applied thinly and uniformly to prepare a poultice sample, and the adhesive surface was covered with a polyethylene film. This sample of poultice was placed in an aluminum-coated laminated bag, sealed by heat sealing, and allowed to stand in an environment of 40 ° C. and 75% RH.

Examples 2 to 3 A poultice sample was prepared in the same manner as in Example 1 except that the composition was changed as shown in Table 2, placed in an aluminum-coated laminated bag and heat-sealed to 40. ℃, 75% RH
It was left standing in the environment.

Comparative Examples 1 and 3 A poultice sample was prepared in the same manner as in Example 1 except that the composition was changed as shown in Table 2. The poultice sample was placed in an aluminum-coated laminated bag and heat-sealed. ℃, 75% RH
It was left standing in the environment.

COMPARATIVE EXAMPLE 2 28.5 parts by weight of Polymer 5 (solid content 15% by weight), which is an aqueous solution of polyacrylic acid, was mixed and dispersed in 6 parts by weight of propylene glycol and 20 parts by weight of glycerin to prepare liquid C. A poultice sample was prepared in the same manner as in Example 1 except that the amount of water was reduced to 9.5 parts by weight, placed in an aluminum-coated laminated bag and heat-sealed at 40 ° C. and 75% RH.
It was left standing in the environment.

The poultice samples obtained in the above Examples and Comparative Examples were evaluated for their adhesive properties by the following evaluation methods. The measurement atmosphere was 25 ° C. and 65% RH.

.Adhesiveness (ball tack) Apply 10g of adhesive base to 10cm × 14cm non-woven fabric
After that, cut out a 10 cm long × 5 cm wide test piece,
After standing still at 40 ° C. and 75% RH for 1 day, JISZ 02
It was subjected to 37 tack test methods. Place the adhesive side up on the ball rolling device.
To the top of the test piece with a tilt angle of 30 degrees.
From a position of 10 cm from 1/32 to 31/32 inch
Roll the stainless ball at the initial speed of 0, and on the adhesive for 1 minute
Ball with a value 32 times the diameter of the largest ball to stop
Measured value as a number (BT₁). Also, 40
Ball tack value (BT after standing for 15 days at 75 ℃ and RH)
₂ ) Was also measured by the above method. ・ Daily stability BT above₁ -BT₂ Is.

A 10 g × 14 cm non-woven fabric having a shapeability of 10 g is applied to a non-woven fabric, left standing at 40 ° C. and 75% RH for 1 day, and then manually applied to a pre-weighed SUS304 stainless steel plate. 10 g /
With the load of cm ² still applied, the mixture was allowed to stand at 37 ° C. and 60% RH for 6 hours, peeled off, and the stainless steel plate was weighed to calculate the weight of the adhesive base remaining adhered.・ A poultice sample obtained in the same manner as in the case of exudation from a nonwoven fabric
After standing still at 0 ° C. and 75% RH for 1 day, it was confirmed by touching with a finger whether or not the non-woven fabric pressure sensitive adhesive was exuded on the non-coated surface.

[0048]

[Table 2]

As is clear from Table 2, all the examples of the present invention showed excellent adhesive properties. However, the neutralization rate is 40
% Of polyacrylic acid salt alone, the shapeability and day-to-day stability were poor, and the day-to-day stability was particularly poor in Comparative Example 2 using solution A containing polyacrylic acid as an aqueous solution. Was. Further, in Comparative Example 3 in which the polyacrylic acid powder having a low molecular weight and a low viscosity of 10% aqueous solution was used, the exudation from the nonwoven fabric was observed.

[0050]

EFFECT OF THE INVENTION The adhesive base for poultice of the present invention has excellent adhesive strength, stability over time, and shapeability, and is a high-performance product that does not exude from a nonwoven fabric. This is because the raw material polyacrylic acid or a salt thereof having a neutralization rate of 30 mol% or less has a high molecular weight, and these are dispersed or dissolved in a polyhydric alcohol and then dispersed or dissolved in the polyhydric alcohol. This is due to a synergistic effect such that the mixing with the monovalent acrylic acid salt is first brought into contact with the aqueous solution or dispersion of the polyvalent metal compound. The adhesive base for poultice of the present invention is useful as a poultice for anti-inflammatory and analgesia, a transdermal preparation base for other physiologically active substances, and a cooling tool.

─────────────────────────────────────────────────── ─── Continuation of front page (56) References JP-A-60-99180 (JP, A) (58) Fields investigated (Int.Cl. ⁷ , DB name) A61K 9/00 A61K 47/00

Claims (6)

(57) [Claims] 1. Satisfying all of the following adhesive properties , (1) 10 g of adhesive base is applied to a non-woven fabric of 14 cm × 10 cm, and a test piece of 10 cm in length × 5 cm in width is cut out at 40 ° C. and 75%. After standing still for 1 day in RH, JIS Z
The ball tack value BT ₁ at an inclination angle of 30 ° when the test was carried out according to the tack test method of 0237 is the ball number 2
It is 0 or more. (2) After applying 10 g of the adhesive base to a non-woven fabric of 14 cm × 10 cm, a test piece of 10 cm in length × 5 cm in width is cut out, and allowed to stand at 40 ° C. and 75% RH for 15 days.
Inclination angle of 30 according to the tack test method of 0237
The ball tack value BT _{2 in} degrees is the ball number 13 or more. (3) The above BT ₁ -BT ₂ is 8 or less. (4) Apply 10 g of adhesive base to a 14 cm × 10 cm non-woven fabric, leave it at 40 ° C., 75% RH for 1 day, and 15
After left standing for a day, it is attached to a stainless steel plate of SUS304.
With a load of 10g / cm ² applied , 37 ℃, 60% R
The weight of the pressure-sensitive adhesive base remaining on the stainless steel plate when it was peeled off after being left to stand for 6 hours in H was all less than 0.2 g. Moreover, the weight average molecular weight in the polyhydric alcohol is 1 × 1.
Solid polyacrylic acid of 0 ⁶ or more and / or neutralization rate
Solid state of 30 mol% or less (0% is not included, the same below)
Neutralize with dispersed or dissolved polyacrylate
Polyacrylic acid monovalent salt with a ratio of 40 to 100 mol%
Polyvalent metallized by dispersing or dissolving in rucor
A pressure-sensitive adhesive base for a polyacrylic acid-based poultice, which is a mixture with water containing a compound. 2. Satisfying all of the following adhesive properties, (1) 10 g of adhesive base into 14 cm × 10 cm non-woven fabric
After application, cut out a test piece measuring 10 cm in length and 5 cm in width
Then, after leaving still at 40 ° C. and 75% RH for 1 day, JIS Z
Inclination angle when performed according to the tack test method of 0237
The ball tack value BT ₁ at 30 degrees is the ball number 2.
It is 0 or more. (2) 10g adhesive base on 14cm × 10cm non-woven fabric
After application, cut out a test piece measuring 10 cm in length and 5 cm in width
Then, after leaving still at 40 ° C. and 75% RH for 15 days, JIS Z
Inclination angle of 30 according to the tack test method of 0237
The ball tack value BT _{2 in} degrees is less than or equal to the ball number 13.
Above. (3) The above BT ₁ -BT ₂ is 8 or less. (4) 10g adhesive base on 14cm × 10cm non-woven fabric
Apply and leave at 40 ° C, 75% RH for 1 day, and 15
After left standing for a day, it is attached to a stainless steel plate of SUS304.
With a load of 10g / cm ² applied, 37 ℃, 60% R
For a stainless steel plate when peeled after standing still for 6 hours
If the weight of the adhesive base remaining after adhesion is less than 0.2 g,
is there. And in a polyhydric alcohol, in a 10% aqueous solution
Polyacrylic acid with a viscosity of 1500 cps or more and /
Alternatively, disperse polyacrylate having a neutralization rate of 30% or less.
Is a dissolved one and a polycondensation ratio of 40 to 100 mol%
Disperse or dissolve acrylic acid monovalent salt in polyhydric alcohol
What was mixed with water containing polyvalent metal compound
A polyacrylic acid-based adhesive for poultices characterized by being
Base agent. 3. A polyhydric alcohol having a C number> OH number ≧ 2.
And linear polyacrylic acid and / or medium
A polyacrylic acid salt having a sum ratio of 30 mol% or less is used.
The adhesive base according to 1 or 2 . 4. The method for producing an adhesive base according to claim 1.
There is a weight average molecular weight of 1 x 10 in the polyhydric alcohol.
⁶ Above solid polyacrylic acid and / or neutralization rate 3
Disperse or dissolve 0 mol% or less of solid polyacrylate.
Of polyacrylic acid monovalent salt and polyvalent alcohol
A polyvalent metal compound dispersed or dissolved in
Poria characterized by being mixed in the presence of water containing
A method for producing an adhesive base for a krill type poultice. 5. The method for producing an adhesive base according to claim 2.
Therefore, the viscosity of 10% aqueous solution in polyhydric alcohol
Polyacrylic acid with a degree of 1500 cps or higher and / or
Is a polyacrylate having a neutralization rate of 30% or less
Of polyacrylic acid monovalent salt and polyvalent alcohol
A polyvalent metal compound dispersed or dissolved in
Poria characterized by being mixed in the presence of water containing
A method for producing an adhesive base for a acrylic acid type poultice. 6. A polyhydric alcohol having a C number> OH number ≧ 2.
And linear polyacrylic acid and / or medium
A polyacrylic acid salt having a sum ratio of 30% or less is used.
The method for producing the adhesive base according to claim 4 or 5.