JPS63277259A - Flame-retardant for halogen-containing vinyl resin and production thereof - Google Patents

Abstract

PURPOSE:To obtain the titled flame retardant applicable to a halogen-containing vinyl resin without deteriorating the transparency, thermal stability, thermal aging resistance, etc., of the base resin, by compounding specific amounts of an alkali metal compound, etc., to antimony pentoxide. CONSTITUTION:100pts.wt. of antimony pentoxide (Sb2O5) is compounded with (A) 3-25pts.wt. of an alkali metal hydroxide (in terms of M2O wherein M is Na or K), (B) 2-33pts.wt. of one or more compounds selected from alkaline earth metal compounds, zinc compound and lead compounds which are one or more compounds selected from hydroxides, oxides, etc. (in terms of M'O wherein M' is Mg, Ca, etc.) and (C) 0.1-8pts.wt. of a perchloric acid compound (e.g. sodium perchlorate) (in terms of ClO4). The molar ratio of (A+B)/Sb2O5 is 0.7-2. If necessary, the obtained mixture is further compounded with (D) 1-5pts.wt. of an organic acid (e.g. maleic acid) and (E) 0.1-3pts.wt. of phosphoric acid (in terms of P2O5). The obtained composition is dried and pulverized to form a powdery flame-retardant having particle diameter of 0.2-10mu.

Description

Detailed Description of the Invention (Field of Industrial Application) The present invention relates to a flame retardant for halogen-containing vinyl resin containing antimony pentoxide as a main component and a method for producing the same. Antimony pentoxide (S), which does not impair the transparency and thermal stability of the resin.
The present invention relates to a flame retardant for halogen-containing vinyl resins whose main component is b2O2) and a method for producing the same.

(Prior art) Halogen-containing vinyl resins themselves have good flame retardancy, but for example, so-called soft vinyl chloride resins plasticized with a plasticizer such as dioctyl phthalate, or halogen-containing resins blended with flammable resins. Vinyl resin burns easily. Soft PVC products such as leather, canvas, electric wires, films, and sheets, which are widely used as automobile interior materials, electrical and electronic parts, and construction materials, or soft PVC products containing impact reinforcement materials are particularly flame-retardant. ization is essential.

Various flame retardants are used to make these resins flame retardant. Inorganic substances such as antimony trioxide (SbzC)s), sodium antimonate, aluminum hydroxide, zirconium oxide, zinc borate, and borax, and organic compounds such as tricresyl phosphate, trichloroethyl phosphate, and chlorinated paraffin are used. . Also, organic bromine flame retardants are rarely used. These include flame retardant effect, transparency,
It has advantages and disadvantages in terms of heat stability, heat aging resistance, weather resistance, cold resistance, bleed/bloom resistance, etc.

Antimony trioxide exhibits excellent flame retardancy, but it usually has a particle size of about 0.5 to 10 μm, has a large refractive index, and has low light transmittance, so it has extremely high hiding properties. Transparency, which is the most important characteristic of resin, is completely lost. Furthermore, when coloring is carried out by adding a pigment, there are drawbacks such as a large amount of pigment being required for the concealing property, and the types of colors that can be obtained being limited.

In order to improve this drawback, it has been proposed to make the particle size extremely small (Japanese Patent Publication No. 45-1435'8) or to increase the particle size by forming a single crystal. Both of these methods are used to improve light transmittance, and the former method significantly improves transparency, but when pigments are added, the hiding power is large and the thermal stability of the resin is deteriorated. , and the cost is high. Furthermore, the latter method does not provide sufficient transparency.

Aluminum hydroxide, zirconium oxide, boric acid, zinc,
Inorganic substances such as borax have inferior flame retardant effects compared to antimony trioxide, and also lose transparency, similar to antimony trioxide. Phosphorous plasticizers such as tricresyl phosphate, which do not lose the transparency of the resin and have a plasticizing effect, and chlorinated paraffin have inferior flame retardant effects to antimony dioxide, so they must be added in large amounts. As a result, it tends to bleed and has poor cold resistance.

Antimony pentoxide is an antimony-based flame retardant that can be applied to halogen-containing vinyl resins and does not impair the transparency of the resin. (Journal Coated Fabric Vol. 11, p. 137 Published in 1982 (J, Coated Fabric
ic Vot, 11. P, 137.1982)) *This is antimony pentoxide sol (particle system 20-100rnμ
) is powdered by spray drying etc., and is antimony pentoxide tetrahydrate. Antimony pentoxide tetrahydrate has a small refractive index and its secondary particles are extremely small, so it has a high light transmittance and has very good transparency. However, antimony 205 oxide has the major drawback of significantly deteriorating the thermal stability of the resin (
(see comparative example). To compensate for this drawback, Ba-Cd-Z
The use of n-type stabilizers or tin mercaptide-type stabilizers has been proposed (Journal of Coated Fabrics, Vol. 11, p. 137, published in 1982 (J, Coated Fabrics).
d Fabric Vol. 11. P, 137.19
82)). However, the former cannot be used in practice because of the toxicity of cadmium and the occurrence of bleed bloom, while the latter has poor weather resistance.

The present inventors have conducted research on flame retardants that do not have the above-mentioned drawbacks, and have already proposed an antimony pentoxide-based flame retardant that has improved these drawbacks in JP-A-60-58453. This includes alkali metals, alkaline earth metals and/or zinc, lead,
In particular, it was possible to significantly improve the thermal stability with antimony pentoxide containing organic acids, phosphoric acid and/or alkali phosphate salts.

However, even with this improved antimony pentoxide flame retardant, sufficient flame retardance cannot be obtained when added in small amounts, and when the amount added is increased to improve flame retardance, thermal stability, heat aging resistance, weather resistance etc. It became clear that there was a tendency for the value to decrease slightly.

In recent years, as demand for halogen-containing vinyl resins has diversified, demand for flame-retardant halogen-containing vinyl resins with excellent transparency and coloring properties has been increasing.

(Problems to be Solved by the Invention) In order to meet this demand, the present inventors have conducted extensive research on antimony pentoxide-based flame retardants that have further improved the above-mentioned drawbacks, and as a result, have completed the present invention. . That is, the present inventors have found that when antimony pentoxide is applied to a halogen-containing vinyl resin, it takes advantage of the characteristic that it does not impair the transparency of the resin, but on the other hand, it deteriorates the thermal stability, heat aging resistance, and weather resistance of the resin. Various studies were conducted to overcome this drawback.

Unlike antimony trioxide, antimony pentoxide is a fairly strong solid acid, so it contains Na, Mg, and Ca.

S r , B a + Z n * Cd + P b
It has the property of strongly binding with basic substances such as oxides, hydroxides, and salts with weak acids. Therefore, if antimony pentoxide is used as it is as a flame retardant, it will react with metal soaps used as stabilizers, such as zinc stearate, barium stearate, etc., and its function as a stabilizer will be significantly reduced. As a result, the thermal stability of the plasticized halogen-containing vinyl resin deteriorates, and coloring and
It is assumed that this causes a bleed bloom phenomenon.

Based on the above facts and reasoning, the present inventors first added Na, Ca, and Mg to antimony pentoxide colloid.

Sr, Ba, Zn, A/i! , Sb, and (III) in the form of oxides, hydroxides, and salts, singly or in combination, and the resulting composition is applied to a plasticized halogen-containing vinyl resin. Its thermal stability was measured.

As a result, we found that a combination of alkali metals and alkaline earth metals and/or Zn, Pb, etc. is effective in improving thermal stability. Since it was not possible to sufficiently improve the properties, the addition of a third component was considered.

Japanese Patent Publication No. 57-47926 describes carboxylates or ferulates of Group 1 and Group Ⅰ metals (commonly used metal soap stabilizers belong to this category), basic inorganic acid salts, and halogen oxygen. It is stated that by adding an acid salt to a halogen-containing resin, deterioration of the resin due to light and heat can be prevented.

Halogen-containing resins using the above metal carboxylates, basic inorganic acid salts, and halogen oxyacids as stabilizers and adding antimony pentoxide have higher thermal stability than ordinary metal soap stabilizers alone. Although the initial colorability is slightly improved, from the viewpoint of practical use, all of the thermal stability, heat aging resistance, and initial colorability are still insufficient.

As mentioned above, the present inventors added an alkali metal hydroxide, an alkaline earth metal and/or Z to antimony pentoxide colloid.
By further adding perchlorate to the composition made alkaline by adding n, Pb hydroxide, oxide or salt,
It has been found that this thermal stability, heat aging resistance, and initial coloring property can be surprisingly improved.

An object of the present invention is to provide a flame retardant that does not impair the transparency of a halogen-containing vinyl resin and does not reduce the thermal stability, heat aging resistance, initial coloring property, and weather resistance of the resin, and a method for producing the flame retardant.

(Means for solving the problems) The present invention provides antimony pentoxide (S bzoS) i o o
The following A to C (A) 3 to 25 parts by weight of an alkali metal compound with the general formula MtO (M=Na, K) as essential components per part by weight, (B) an alkaline earth metal compound, a zinc compound, and At least one compound selected from lead compounds is represented by the general formula M
'O(M'=Mg, Ca, Sr, Ba, Zn.

The present invention relates to a powdery flame retardant for halogen-containing vinyl resins, characterized in that it contains 2 to 33 parts by weight as Pb) and 0.1 to 8 parts by weight as (C) perchloric acid.

The present invention will be explained in more detail below. The antimony pentoxide used in the present invention can be obtained by the method of oxidizing antimony trioxide (Japanese Patent Publication No. 57-11848), or by the method of dealkalizing alkali antimonate with an ion exchange resin (U.S. Pat.
1'l O247), a method of peptizing after reacting an alkali antimonate with an inorganic acid (Japanese Patent Application Laid-Open No. 60-4153)
It is an antimony pentoxide suspension obtained by acid-treating antimony pentoxide sol and sodium antimonate having a primary particle size of 5 to 100 mμ, which are produced by a method such as No. 6, JP-A No. 61-227918). Furthermore, antimony pentoxide used in the present invention is known to be a strong cation exchanger (Japanese Patent Publication No. 45-6695). The antimony pentoxide produced by the above method has S b toscN a 20
)X-4H2O, generally x=0~
Since it is 0.4, the added alkali metal ion,
It has the property of strongly adsorbing alkaline earth metal ions and zinc ions, and incorporating them into its structure. Therefore, by adding soluble hydroxides or soluble salts of alkali metal hydroxides, alkaline earth metals, zinc and lead to antimony pentoxide sol and antimony pentoxide suspension, the cation exchange ability of antimony pentoxide can be improved. It can be blocked. Particularly effective is sodium hydroxide.

Surprisingly, (M2O+M'0)/S b
Even if the tos molar ratio is 0.8 or more, it retains the antimony pentoxide tetrahydrate structure and does not become a salt such as sodium antimonate. Furthermore, the cation exchange ability can be blocked by using a hydroxide with low solubility instead of the above-mentioned soluble salt.

By adding an alkali metal compound, an alkaline earth metal compound, etc., the antimony pentoxide sol undergoes micro-agglomeration and becomes a modified antimony pentoxide slurry. When soluble salts such as chlorides are used, unnecessary anions such as chlorine must be removed by washing or ion exchange. Since the obtained modified antimony pentoxide slurry contains a base having more than ion exchange capacity, p f
(is 7 to 12.

This modified antimony pentoxide mainly has sodium ions in its structure, and alkali ions other than sodium,
It is presumed that alkaline earth ions, Zn ions, etc. are bound to the surface. Furthermore, it is presumed that antimony pentoxide colloid is strongly adsorbed or bound to the surface of insoluble oxides and salts, such as magnesium oxide, basic zinc carbonate, and zinc oxide.

The method for producing the flame retardant of the present invention is to add the above-mentioned components A to C as solids to the above-mentioned antimony pentoxide sol or antimony pentoxide suspension so as to have the above-mentioned composition, and then to separate the solids. Alternatively, the product can be produced by drying as it is and pulverizing the dried product after drying.

As the alkali metal compound of component A, hydroxide (Na
OH, KOH), water-soluble salts (NaC1°K(1)
etc. can be used. Among these alkali metal compounds, hydroxides are preferred, and caustic soda is particularly preferred. The alkaline earth metal compounds, zinc compounds and lead compounds of component B include hydroxides (Mg(OH)z, Ca(OH)z, 5
r(OH)z, Ba(OH)z'882O, Zn(OH
)z, Pbo-nHzo, etc.), oxides (MgO, Cab
, SrO, Bad, ZnO.

pbo, etc.), water-soluble salts (M g C-i! z +
Ca Cl z.

SrC/! , BaC1z, ZnCf□Zn5Oa+Pb
CN03h, etc.), carbonates (MgCO:+, MgCa(C
Os) z+ Ca COs-S r C03+ B
a COs, Z nCO5, Pb, COs, etc.), basic salt (Mg(OH)z・3MgCC)+, 3 Zn(O
H)z・2 ZnC0z, P b(OH)z・2
PbCC)+, Zn(OH)C,i! etc.), etc.) can be used.

The perchlorate of component C is NaCl0a and KCl.

04, Mg(CfOn)z, CaCCl0a)z+
5r(CI!o4)z+ Ba(Cj!04)z, Zn
(CI!, OJz, etc. can be used.

Any type of perchlorate can be added in the present invention, but since sodium and potassium perchlorates are oxidizing agents and have the risk of explosion, the perchlorate produced should not be anything other than an alkali metal salt. is preferred.

That is, it is necessary to react the alkaline earth metal compound, zinc compound, and lead compound with perchlorate ions in the modified antimony pentoxide slurry. for example,
When sodium perchlorate is added in the presence of a large amount of barium hydroxide, sodium ions are incorporated into antimony pentoxide, producing barium perchlorate, and sodium perchlorate is added in the presence of a large amount of basic zinc carbonate. The perchlorine ions then react with basic zinc carbonate to partially form basic zinc perchlorate or zinc perchlorate.

Furthermore, in addition to the above formulations, organic acids such as maleic acid, citric acid, malonic acid, phthalic acid, fumaric acid and stearic acid and/or Alternatively, phosphoric acid may be added. The blending amounts of these compounds are 1 to 5 parts by weight of organic acid and 0.1 to 3 parts by weight of phosphoric acid as PtOs per 100 parts by weight of antimony pentoxide.

Note that the addition of the alkali metal compound, alkaline earth metal compound, etc., perchlorate, etc. can be carried out at room temperature to 100° C., and strong stirring such as in a disper is preferable.

The solid content in the antimony pentoxide-based flame retardant slurry thus obtained is separated, or directly evaporated to dryness, or dried using a spray dryer, drum dryer, freeze dryer, or the like. The drying temperature at this time is not particularly limited, but it is sufficient that free water can be removed within a range where the product temperature does not exceed around 200°C at maximum. The solid content can be separated by conventional methods such as filtration and centrifugation. After this drying, the flame retardant of the present invention can be obtained by pulverizing the dried product as necessary to form a powder. The pulverization is preferably performed using a bin disc mill, a high-speed rotation mixer, a jet oomizer, or the like.

The above-mentioned barium perchlorate, zinc perchlorate, etc. are generated during the drying process, and it is assumed that these are strongly adsorbed or bonded to the surface of the antimony pentoxide colloid, and are also very uniformly dispersed. It is estimated that

In addition, this powder has a particle size of 0.2 to 10μ,
Even if it is 10μ or more, it has the characteristic that it can be easily pulverized when mixed with vinyl chloride resin using a Henschel mixer or the like.

The flame retardant of the present invention is a halogen-containing vinyl resin, a plasticizer, B
After mixing the a-Zn stabilizer with a Henschel mixer, 1
A wire sheet with a thickness of 0.7 to 0.8 mm was produced using two rolls at 70°C.

The gear oven method was adopted as a test method for the thermal stability of this sheet. The oven temperature was set at 185°C, and thermal stability was evaluated based on the time taken for the test piece to blacken and the degree of initial coloration.

According to the above test method, the initial coloring is smaller when component A and at least one of the alkaline earth metal compounds, zinc compounds, and lead compounds of component B are mixed than when the alkali metal compound of component A is alone.

Furthermore, the addition of the above-mentioned component C, a perchloric acid compound, has a remarkable effect on preventing initial discoloration, improving thermal stability, and improving heat aging resistance.

The blending amounts of these components A to C are as described above, but in the flame retardant, the alkali metal compound of component A is expressed as an oxide of the general formula M, based on 100 parts by weight of antimony pentoxide (S btos). 3-15% by weight as O(M-Na, K)
, at least one compound selected from alkaline earth metal compounds, zinc compounds, and lead compounds as component B is expressed by the general formula M'0 (M/= M g .

2 to 33 parts by weight as Ca, Sr, Ba, Zn, Pb), 0.1 to 8 as 0204 perchloric acid compound of C component
parts by weight, and if necessary, 1 to 5 parts by weight of (D) organic acid, and/or 0.1 to 3 parts by weight of (E) phosphoric acid as P2Os. Furthermore, the blending amounts of component A and component B are (M!O+M'O)/S with respect to antimony pentoxide.
The molar ratio of b2OS to bgos is preferably in the range of 0.7 to 2. If it is less than 0.7, it is insufficient to suppress the ion exchange ability of antimony pentoxide, and if it is more than 2, excess base or basic substances remain, which promotes dehalogenation of the halogen-containing vinyl resin and prevents initial coloring. It gets bigger and I don't like it.

Among component B, basic zinc carbonate can prevent initial coloring of the resin and significantly improve thermal stability and heat aging resistance. In the case of antimony trioxide, addition of such basic zinc carbonate causes zinc burning, and blackening occurs in a significantly short period of time. In the case of antimony pentoxide, the acidity of antimony pentoxide and the basicity of basic zinc carbonate can be balanced, so it is presumed that more basic zinc carbonate can be added than is commonly thought possible.

The thus obtained flame retardant of the present invention is added to a halogen-containing vinyl resin, a plasticizer such as dioctyl phthalate, Ba-Z
The method of blending with additives such as n-type stabilizer and epoxidized soybean oil is a known method. For example, halogen-containing vinyl resin, powder stabilizer, and flame retardant are mixed, and while stirring with a Henschel mixer, epoxidized Add dioctyl phthalate (DOP) dissolved in soybean oil in advance,
This is carried out by mixing until the temperature reaches 05 to 115°C. At this time, the amount of the flame retardant of the present invention is 0.5 to 20 parts by weight per 100 parts by weight of the halogen-containing vinyl resin.

In the present invention, halogen-containing vinyl resin means vinyl chloride resin and copolymers thereof. Copolymers with vinyl chloride resins include copolymers of ethylene, propylene, vinylidene chloride, vinyl acetate, vinyl alcohol, acrylic esters, methacrylic esters, styrene, acrylonitrile, etc., and vinyl chloride graft copolymers. Examples include graft copolymers of polystyrene with vinyl acetate, polyesters, polyurethanes, polystyrene, and the like. A copolymer as used herein refers to a polymer containing two or more types of monomers.

The flame retardant of the present invention is a flame retardant for halogen-containing vinyl resin that does not impair the transparency of the halogen-containing vinyl resin, nor does it deteriorate the thermal stability, heat aging resistance, initial coloring property, and weather resistance.

EXAMPLES The present invention will be specifically explained below with reference to Examples, but the present invention is not limited thereto.

Note that the composition percentages in Examples and Comparative Examples are expressed in weight percent.

Example 1 Antimony pentoxide sol (s
b, o, 17°4%, Na2O1.16%, P2O°0
．． 22%, pH 2,0) 3870g of Mg(OH)zl
3.6 g, Ba(OH)z ・8Hz0 36.
After adding 4 g and stirring with a disper for 1.5 hours, 70.7 g of 93% NaOH, 60% Na C120
After stirring and dissolving, 80.4 g of basic zinc carbonate was added and the mixture was further stirred for 1 hour. The pH of the resulting slurry was 0.0. This slurry was dried at 130° C. for 6 hours, and the resulting dried product was ground with a pin disc mill. The average particle size of the obtained flame retardant powder was 3μ.

Example 2 A sol (S
b z Os 21.4%, Na2O2.70%.

P2Oso, 14%, pH 6,5) 99 to 1060 kg
%NaOH8, 13kg, 60% NaClO4 aqueous solution9
．． After adding 87 kg and stirring for 1 hour with a disper, 14.24 kg of basic zinc carbonate was added, and further 1
Stir for hours. The obtained slurry was dried with a spray dryer to obtain a powder. The average particle size of this product was 15μ.

Example 3 Antimony pentoxide sol (S
btO515%, Natoo, 95%, pH2,1)5
70kg contains 99% NaOH8.21kg, Ba(OI(
)Z.8H2O (5,83 kg) was added, and the mixture was stirred with a disper for 1.5 hours, and then 3,72 kg (3,72 kg) of a 60% Na Cl O4 aqueous solution was added, and the mixture was further stirred for 30 minutes. The obtained slurry was dried with a spray dryer to obtain a powder. The average particle size of this product was 15μ.

Example 4 Antimony pentoxide sol (sb
, os 13.3%, Natal. 04%, pH2,
5) 650 kg, 10% NaOH aqueous solution 17.1 kg, stearic acid 1.73 kg, isopropanol 1.1 k
After adding g and stirring with a disper for 1.5 hours,
a (OH)z '8H, 034゜15kg, 85%
Added 419 g of phosphoric acid and 13.2 kg of basic zinc carbonate, and further added 1.7 g of 60% Na CIt O4 aqueous solution.
kg was added and stirred for 2 hours.

Dry the obtained slurry with a spray dryer,
Further, this dried product was pulverized in a bottle disc mill to obtain a powder with an average particle size of 3 μm.

Comparative Example 1 Antimony pentoxide sol (S
bios 12%, Na2O0.80%, pH2゜5)
4.1 g of 93% NaOH and 16 g of Ba(OH).8 H2O were added to 600 g, and the mixture was stirred in a disper for 4 hours. The obtained slurry was passed through a suction port, and the wet cake was dried at 150° C. for 4 hours.The dried product was then ground with a pin disk mill to obtain a powder. The average particle size of this powder was 3μ.

Comparative Example 2 Antimony pentoxide sol (Sb
2OslO%, Na2Oo, 57%, pH2゜3)7
Zn(OH)zl 5g, Ba(OH)z in 20g
・After adding 016 g of 8H and stirring for 2 hours using a disper, 3° og of maleic acid and 25 g of an io% HsPOa aqueous solution were added, and the mixture was further stirred for 2 hours. The resulting slurry was separated daily through a suction port to obtain a wet cake, which was dried at 170° C. for 3 hours, and this dried product was pulverized with a pin disk mill. The average particle size of the obtained powder was 3μ
Met.

Comparative Example 3 Antimony pentoxide sol (Sb2
Os12%, Na, 2O0.83%, pH2,3)10
Add 15g of 93% NaOH to 00g and mix with a disperser.
Stir for 5 hours, then add 60% Na Cj204 aqueous solution 5 hours.
．． Og was added and the mixture was further stirred for 2 hours.

The resulting slurry was evaporated to dryness at 130°C and ground in a pin disc mill. The average particle size of the obtained powder was 3μ.

[Evaluation of flame retardants]

The test method is as follows.

Thermal stability (blackening time): The test pieces were mixed in a Henschel mixer according to the recipe (■) at 170°C (a sheet with a thickness of 0.7 to 0.8 mm was created using 712 rolls, and the oven temperature was 185°C). The time to blackening was measured.

Initial colorability (YI value): The color difference of the test piece was measured by the reflected light of a 1 mm thick press sheet prepared according to formulation ①, and the colorability was shown by YI value (Yellow value).

Transparency: The test piece was prepared by measuring the transmittance (L value) of a 1 mm thick press sheet using transmitted light.

Bleeding property: The test piece was determined by a method in which a 1 mm thick press sheet prepared according to the formulation (1) was left at 80° C. and a humidity of 99% for 7 days, and visually observed whether liquid oozed out from the sheet surface.

Judgment criteria ○: No bleeding Δ: Slight bleeding ×: Bleeding Heat aging properties: Test pieces are 0.5 mm prepared according to the formulation ■
A press sheet was prepared, and 4
After hanging for 00 hours, the residual percentage of tensile elongation was determined.

Light resistance: A 0.2 tm film was prepared as a test piece according to Formulation I, and the residual percentage of tensile elongation was determined after irradiation with QUV for 210 hours.

QUV: DPWL-5R type (Suga Test Instruments ■) Irradiance: 3.9 mW/cm" Black panel temperature;
71°C Wet temperature = 47°C Flame retardancy: Carbonization length and afterflame were measured according to the vertical combustion test method of JIS L-1091. As a test piece, a canvas having a thickness of 0.37 mo+ was prepared according to the formulation (2).

Oxygen index: Measured according to JIS K 7201. A 3 mm film was prepared as a test piece according to formulation (2).

The PVC formulations used in the above test method were prepared according to the four formulations shown in Table 1.

The composition of the flame retardant produced above is shown in Table 2, and the evaluation results are shown in Table 3. The moisture content in Table 2 is based on differential thermal analysis.

(Left below) Table-1 Combination prescription ll1111IV PV C (P=1000) 10010010010
0 possible a) DOP 40
50 50 plastic rJ) TCP 1
0,

Claims (19)

[Claims] (1) The following A to C (A) alkali metal compounds with the general formula M_2O (M=Na
, 3 to 25 parts by weight as K), (B) at least one compound selected from alkaline earth metal compounds, zinc compounds, and lead compounds with the general formula M
Contains 2 to 33 parts by weight as 'O (M' = Mg, Ca, Sr, Ba, Zn, Pb), 0.1 to 8 parts by weight of (C) perchloric acid as ClO_4, and if necessary, the following: A powdery flame retardant for halogen-containing vinyl resin, characterized in that it contains 1 to 5 parts by weight of D and/or E (D) an organic acid, and 0.1 to 3 parts by weight of (E) phosphoric acid as P_2O_5. (2) Halogen-containing according to claim 1, wherein the amount of component A and component B is in the range of 0.7 to 2 in molar ratio of (M_2O+M'O)/Sb_2O_5 to antimony pentoxide. Flame retardant for vinyl resin. (3) The flame retardant for halogen-containing vinyl resins according to claim 1, wherein the alkali metal compound is a hydroxide. (4) The halogen according to claim 1, wherein the alkaline earth metal compound is at least one compound selected from hydroxides, oxides, water-soluble salts, carbonates, and basic salts. Contains flame retardant for vinyl resin. (5) The halogen-containing vinyl resin according to claim 1, wherein the zinc compound is at least one compound selected from hydroxides, oxides, water-soluble salts, carbonates, and basic salts. Flame retardant for use. (6) The flame retardant for halogen-containing vinyl resins according to claim 5, wherein the zinc compound is basic zinc carbonate. (7) The halogen-containing vinyl resin according to claim 1, wherein the lead compound is at least one compound selected from hydroxides, oxides, water-soluble salts, carbonates, and basic salts. Flame retardant for use. (8) The perchloric acid compound is at least one selected from sodium perchlorate, potassium perchlorate, magnesium perchlorate, calcium perchlorate, strontium perchlorate, barium perchlorate, and zinc perchlorate. The flame retardant for halogen-containing vinyl resins according to claim 1, which is a seed compound. (9) For the halogen-containing vinyl resin according to claim 1, wherein the organic acid is at least one compound selected from maleic acid, citric acid, malonic acid, phthalic acid, fumaric acid, and stearic acid. Flame retardants. (10) The flame retardant for halogen-containing vinyl resins according to claim 1, wherein the flame retardant is a powder having a particle size of 0.2 to 10 μm. (11) Antimony pentoxide (Sb_2O_5) 10 in antimony pentoxide sol or suspension of antimony pentoxide
The following A to C (A) alkali metal compounds are used as essential components based on 0 parts by weight of the general formula M_2O (M=Na
, 3 to 25 parts by weight as K), and (B) at least one compound selected from alkaline earth metal compounds, zinc compounds, and lead compounds of the general formula M.
Adding 2 to 33 parts by weight as 'O (M' = Mg, Ca, Sr, Ba, Zn, Pb), then adding 0.1 to 8 parts by weight as (C) perchloric acid compound as ClO_4, If necessary, add and mix the following D and/or D (D) 1 to 5 parts by weight of organic acid and (E) 0.1 to 3 parts by weight of phosphoric acid as P_2O_5, and separate the obtained solid content. 1. A method for producing a halogen-containing flame retardant for vinyl wood, which comprises drying the flame retardant or drying it as is, and pulverizing the dried product if necessary after drying. (12) Halogen-containing according to claim 11, wherein the amount of component A and component B is in the range of 0.7 to 2 in molar ratio of (M_2O+M'O)/Sb_2O_5 to antimony pentoxide. A method for producing a flame retardant for vinyl resin. (13) The method for producing a flame retardant for a halogen-containing vinyl resin according to claim 11, wherein the alkali metal compound is a hydroxide. (14) The alkaline earth metal compound is a hydroxide, an oxide,
Claim 11 is at least one compound selected from water-soluble salts, carbonates, and basic salts.
A method for producing a flame retardant for a halogen-containing vinyl resin as described in . (15) Zinc compound is hydroxide, oxide, water-soluble salt,
The method for producing a flame retardant for a halogen-containing vinyl resin according to claim 11, wherein the flame retardant is at least one compound selected from carbonates and basic salts. (16) The method for producing a flame retardant for a halogen-containing vinyl resin according to claim 15, wherein the zinc compound is basic zinc carbonate. (17) The halogen-containing vinyl resin according to claim 11, wherein the lead compound is at least one compound selected from hydroxides, oxides, water-soluble salts, carbonates, and basic salts. method for producing flame retardants for use in (18) The perchloric acid compound is at least one selected from sodium perchlorate, potassium perchlorate, magnesium perchlorate, calcium perchlorate, strontium perchlorate, barium perchlorate, and zinc perchlorate. The method for producing a flame retardant for halogen-containing vinyl resin according to claim 11, which is a seed compound. (19) Claim 11, wherein the organic acid is at least one compound selected from maleic acid, citric acid, malonic acid, phthalic acid, fumaric acid, and stearic acid.
A method for producing a flame retardant for a halogen-containing vinyl resin as described in .