CN107915918B - Flame-retardant double-layer plate for space leasing and preparation method thereof - Google Patents
Flame-retardant double-layer plate for space leasing and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/04—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C08L27/06—Homopolymers or copolymers of vinyl chloride
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/16—Articles comprising two or more components, e.g. co-extruded layers
- B29C48/18—Articles comprising two or more components, e.g. co-extruded layers the components being layers
- B29C48/21—Articles comprising two or more components, e.g. co-extruded layers the components being layers the layers being joined at their surfaces
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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Abstract
The invention discloses a flame-retardant double-layer plate for space leasing and a preparation method thereof, wherein the flame-retardant double-layer plate comprises a first material and a second material which are co-extruded and molded; wherein, the first material and the second material both contain the flame-retardant smoke suppressant, wherein, the weight content of the flame-retardant smoke suppressant in the first material is 20-200% higher than that of the second material; wherein the flame-retardant smoke suppressant is prepared by reacting a compound having R as shown in formula (I)1And R2The substituted phosphinate, tributyltin and tri-n-octylphosphine oxide are heated and contacted at the temperature of 200-300 ℃ to prepare the compound. The flame-retardant smoke inhibitor in the board does not lose flame-retardant property in the high-temperature processing process, does not generate brittle substances, has good mechanical property, is flame-retardant and environment-friendly, and has high popularization and application values.
Description
Technical Field
The invention relates to a flame-retardant sheet material, in particular to a flame-retardant double-layer sheet material for space leasing and a preparation method thereof.
Background
With the development of economic society and the acceleration of pace of life and work, most office areas are no longer fixed reinforced concrete houses, and more office spaces are divided in a building, and the office spaces are rented to target customers in a renting mode. Since these spaces often contain a large number of people, fire resistance is the most important requirement for rental space. Common flame-retardant smoke inhibitors include aluminum hydroxide, cerium hydroxide, magnesium hydroxide, halogen flame-retardant smoke inhibitors, phosphinates, polycyanum and the like, and although the halogen flame-retardant smoke inhibitors commonly used at present are still widely used, the harm to human health and environment is more and more concerned due to the problems of dioxin generation during combustion and toxic gas generation after fire. At present, the phosphinate has the advantages of small dosage, low smoke density, no environmental hazard and the like, and is more and more concerned by people. However, the patent document US 2007/0029532 discloses that phosphonates may cause decomposition during processing and generate brittle unusable substances during processing, thus limiting the use of phosphonates as flame retardant smoke suppressants.
Patent document CN107207779A, entitled: flame retardant polymer compositions comprising heat treated phosphorus compounds and melam disclose that flame retardant smoke suppressants obtained by heating certain phosphonates at 200 ℃ or higher, and melam or melam derivatives as flame retardant synergists, can be readily processed under certain severe conditions by incorporation into the polymer. However, the melam or melam derivatives are not easy to synthesize, so that the application cost of the flame-retardant smoke suppressant added with melam is increased.
Therefore, it is a technical problem to be solved urgently at present how to provide a flame-retardant smoke suppressant and a panel containing the same, which reduce the production cost of the material, improve the flame-retardant performance of the material in the application material, do not produce fragile substances, and do not reduce the influence on the mechanical properties, especially the toughness, of the main material substrate on the basis of ensuring the advantages of low smoke density, no environmental hazard and the like.
Disclosure of Invention
The flame-retardant double-layer board for space leasing contains a flame-retardant smoke suppressant, and the flame-retardant smoke suppressant can improve the flame retardant property of the flame-retardant smoke suppressant in application materials on the basis of keeping the advantages of low smoke density, no environmental hazard and the like of phosphinate, does not generate fragile substances, does not reduce the influence on the mechanical property of a main material matrix, and is more economical in used auxiliaries.
In order to achieve the purpose, the invention provides a preparation method of a flame-retardant double-layer plate for space leasing, which comprises the steps of carrying out co-extrusion molding on a first material and a second material; wherein, the first material and the second material both contain the flame-retardant smoke suppressant, wherein, the weight content of the flame-retardant smoke suppressant in the first material is 20-200% higher than that of the second material; wherein the flame-retardant smoke suppressant is prepared by reacting a compound having R as shown in formula (I)1And R2Substituted phosphinatesTributyltin and tri-n-octylphosphine oxide are heated and contacted at the temperature of 200-300 ℃ to prepare the compound; wherein, in formula (I): r1Is C1-C6 alkyl or phenyl; r2Is C1-C6 alkyl or phenyl; m is a metal and n is a number from 1 to 4, such that Mn+Is a metal cation, where n + represents the charge formally assigned to the cation, and n is a number from 1 to 4.
The invention also provides the flame-retardant double-layer plate for space leasing, which is prepared by the preparation method.
The flame-retardant smoke suppressant in the flame-retardant double-layer plate for space leasing does not lose flame-retardant property in the high-temperature processing process, and the generation of fragile substances is not found, so that the obtained flame-retardant double-layer plate is good in mechanical property, flame-retardant and environment-friendly. The flame-retardant double-layer plate for space leasing can be used for partitioning space to manufacture leasing office space, and can greatly meet the requirements of the existing leasing space on flame retardance, environmental protection and durability. The flame-retardant double-layer plate for space leasing is low in cost, and the manufacturing cost of the leasing space can be indirectly reduced, so that the flame-retardant double-layer plate for space leasing has high popularization and application values.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Detailed Description
The following describes in detail specific embodiments of the present invention. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
The invention provides a flame-retardant smoke suppressant which is represented by the formula (I) and has the R1And R2The substituted phosphinate, tributyltin and tri-n-octylphosphine oxide are prepared after heating and contacting at the temperature of 200-300 ℃; wherein, in formula (I): r1Is C1-C6 alkyl or phenyl; r2Is C1-C6 alkyl or phenyl; m is a metal and n is a number from 1 to 4, such that Mn+Is a metal cation, where n + represents the charge formally assigned to the cation, and n is a number from 1 to 4.
According to the selection of the raw material types and the preparation process of the technical scheme, the flame-retardant smoke suppressant can be obtained by a person skilled in the art. The flame-retardant smoke suppressant provided by the invention can improve the flame retardant property of phosphinate in application materials on the basis of keeping the advantages of low smoke density, no environmental hazard and the like of the phosphinate, does not generate fragile substances, and does not reduce the influence on the mechanical properties of main material matrixes. The flame retardant performance of the flame retardant and smoke suppressant can be improved by the melamine. The preparation raw materials of the flame-retardant smoke suppressant are low in price and easy to obtain, so that the flame-retardant smoke suppressant has higher popularization and application values.
In the above technical scheme, the compound shown as the formula (I) has R1And R2The substituted phosphinate has a relatively mature synthesis method at present, such as a Grignard reagent method, an aluminum chloride catalytic reaction, a free radical addition method, a metal complex catalytic addition method and the like, and all the substituted phosphinate products are commercially available products. Having R as shown in formula (I) in the examples hereinafter in the present invention1And R2The substituted phosphinates were all purchased from Deqing Sihai chemical Co.
The flame retardant smoke suppressant of the present invention can be added to various raw materials for producing polymers such as plastics or rubbers to obtain target materials for improving the flame retardancy of the materials, for example, to materials in which polyolefin homopolymers and copolymers, rubbers, polyesters, epoxy resins, polyurethanes, polyalkylene terephthalates, polysulfones, polyimides, polyphenylene ethers, styrene polymers and copolymers, polycarbonates, acrylic polymers, polyamides, polyacetals, epoxy resins are main substrates.
In the process, the flame retardant smoke suppressant of the invention has R as shown in formula (I)1And R2The substituted phosphinate does not lose flame retardant properties during high temperature processing, and brittle substances are not found to be generated in the applied materials. Hereinafter, the application of the flame retardant and smoke suppressant of the present invention to a material mainly composed of polyvinyl chloride will be described.
In the present invention, in order to obtain the flame retardant and smoke suppressant with excellent flame retardant property, less fragile substances in the processed material and good mechanical properties of the processed material, the temperature of the heating contact is preferably 240-280 ℃.
In order to obtain the flame retardant and smoke suppressant with excellent flame retardant property, less fragile substances in the processed material and good mechanical property of the processed material, more preferably, the heating and contacting conditions comprise: having R as shown in formula (I)1And R2The substituted phosphinate, tributyltin and tri-n-octylphosphine oxide are mixed for 20-30min at the temperature of 240-280 ℃, and then are subjected to heat preservation for 1.5-2.5h at the temperature of 260-280 ℃.
In the present invention, R in the formula (I)1And/or R2May be an alkyl group or a phenyl group substituted with one of various substituents such as one or more of nitro, halo, hydroxy, amino, and the like.
In the present invention, preferably, the alkyl group is an alkyl group which is unsubstituted or substituted by one or more of halogen, hydroxyl, amino.
In the above technical scheme, the type of the alkyl group can be selected in various ways, and can be a straight chain alkyl group or a branched chain alkyl group. The position of the alkyl group substituted by the substituent may be variously selected, and may be substituted at the 1-position or the 2-6-position. And the number of the substituted substituents can be selected in various ways, for example, the invention can be realized by single substitution or multiple substitution.
The position of the phenyl substituted by the substituent can be selected in various ways, and ortho-substitution, meta-substitution and para-substitution can all realize the invention. And the number of the substituted substituents can be selected in various ways, for example, the invention can be realized by single substitution or multiple substitution.
In order to reduce the production of toxic gases containing halogens by high-temperature combustion, it is more preferable that the alkyl group is free of halogen substituents, and the alkyl group is unsubstituted or substituted by one or more of hydroxyl and amino.
In the present invention, preferably, the phenyl group is a phenyl group which is unsubstituted or substituted by one or more of halogen, hydroxyl, amino.
In order to reduce the production of toxic gases containing halogens during high-temperature combustion, it is more preferable that the alkyl group does not contain a halogen substituent, and the phenyl group is an alkyl group which is unsubstituted or substituted by one or more of a hydroxyl group and an amino group.
M of formula (I) may be a conventional metal element, preferably, in order to have R as shown in formula (I)1And R2The substituted phosphinate is cheap and easily available, and preferably, M in the formula (I) is L i, K, Na, Mg, Ca, Ba, Zn, Zr, B, Al, Si, Ti, Sn or Sb.
In the present invention, it is more preferable to have R as shown in the formula (I)1And R2The substituted phosphinate is cheap and easy to obtain, and M is Ca or Al.
In the present invention, the compound represented by the formula (I) has R1And R2Substituted phosphinates, tributyltin andthe weight ratio of tri-n-octyl phosphine oxide can be adjusted in a wide range, and the flame-retardant smoke suppressant can be obtained. In order to obtain the flame-retardant smoke suppressant shown as the formula (I) and having excellent flame-retardant property, less fragile substances in the processed material and good mechanical property of the processed material1And R2The weight ratio of substituted phosphinate, tributyltin and tri-n-octylphosphine oxide is 10: 1-3: 8-10.
The invention also provides a flame-retardant smoke suppressant prepared according to the preparation method of the flame-retardant smoke suppressant.
Through the technical scheme, the flame-retardant smoke suppressant provided by the invention can improve the flame-retardant property of the phosphinate in application materials on the basis of keeping the advantages of low smoke density, no environmental hazard and the like of the phosphinate, does not generate fragile substances, and does not reduce the influence on the mechanical property of a main material matrix. The preparation raw materials of the flame-retardant smoke suppressant are cheap and easy to obtain, so that the flame-retardant smoke suppressant has higher popularization and application values.
The invention also provides a preparation method of the flame-retardant double-layer plate for space leasing, which comprises the steps of carrying out co-extrusion molding on the first material and the second material; wherein, the first material and the second material both contain the flame-retardant smoke suppressant, wherein, the weight content of the flame-retardant smoke suppressant in the first material is 20-200% higher than that of the second material; wherein, the flame-retardant smoke-suppressing agent is the flame-retardant smoke-suppressing agent provided by the invention.
In the process, the flame-retardant smoke suppressant in the flame-retardant double-layer board for space leasing does not lose flame-retardant property in the high-temperature processing process, and the generation of fragile substances is not found, so that the obtained flame-retardant double-layer board is good in mechanical property, flame-retardant and environment-friendly. The flame-retardant double-layer board for space leasing provided by the invention has the advantages that the contents of the flame-retardant smoke inhibitor in the two layers are different, the using amount of the flame-retardant smoke inhibitor can be saved, the production cost is saved, in the using process, the surface with low content of the flame-retardant smoke inhibitor can be used as the non-daily contact surface of the product, and the surface with high content of the flame-retardant smoke inhibitor can be used as the outer surface, so that the product still has good flame retardant property.
And adjusting the size of the roller gap according to the thickness required by processing. And after the full plasticization of the screw rod, the double-layer plate blank is extruded by a narrow-slit machine head. And then the three-roller calender cools and shapes the product, and further cools the product by a guide roller at a certain distance, and then the product can be cut, rolled and molded. The extrusion molding machine is not particularly limited herein, and a conventional extrusion molding machine can be used.
Aiming at the current situation, the flame-retardant double-layer plate for space leasing can be used for dividing space to manufacture leased office space, and can greatly meet the requirements of the existing leased space on flame retardance, environmental protection and durability. The flame-retardant double-layer plate for space leasing is low in cost, and the manufacturing cost of the leasing space can be indirectly reduced, so that the flame-retardant double-layer plate for space leasing has high popularization and application values.
The raw materials in the flame-retardant double-layer plate for space leasing can be adjusted in a wide range, and in order to obtain a plate with good mechanical property and good flame-retardant effect, preferably, the first material comprises the following components in parts by weight: 75-120 parts of polyvinyl chloride, 100 parts of filler, 150 parts of stabilizer, 0.5-1.2 parts of stearic acid, 2-3.5 parts of ACR modifier and 15-25 parts of flame-retardant smoke inhibitor; the second material includes: 75-120 parts of polyvinyl chloride, 100 parts of filler, 150 parts of stabilizer, 0.5-1.2 parts of stearic acid, 2-3.5 parts of ACR modifier and 10-12 parts of flame-retardant smoke inhibitor.
The first and second materials may be obtained by a variety of methods, preferably the first and second materials are prepared by: the polyvinyl chloride, the filling agent, the stabilizing agent, the stearic acid, the ACR modifier and the flame-retardant smoke suppressant are firstly hot-mixed at 140 ℃ and then cold-mixed at 60-80 ℃.
The mixing time of the materials can be adjusted within a wide range by those skilled in the art, and more preferably, the materials are firstly hot mixed at 120-140 ℃ for 1.5-2h and then cold mixed at 60-80 ℃ for 20-40 min.
As for the coextrusion conditions, the skilled person can adjust them within a wide range, preferably the temperature of coextrusion is 160-210 ℃.
And adjusting the size of the roller gap according to the thickness required by processing. And after the full plasticization of the screw rod, the double-layer plate blank is extruded by a narrow-slit machine head. And then the three-roller calender cools and shapes the product, and further cools the product by a guide roller at a certain distance, and then the product can be cut, rolled and molded. The extrusion molding machine is not particularly limited herein, and a conventional extrusion molding machine can be used.
The trade mark for polyvinyl chloride can be adjusted within wide limits by those skilled in the art, and in order to improve the processing effect, it is preferred that the polyvinyl chloride is of the type PVC-SG 5.
The filler can be adjusted within wide range by those skilled in the art, and in order to improve the processing effect, the filler is preferably one or more of heavy calcium carbonate, nano calcium carbonate, perlite, titanium dioxide and light calcium carbonate.
The stabilizer can be adjusted within a wide range by those skilled in the art, and in order to improve the thermal stability of the sheet, it is preferably a lead salt composite stabilizer, an organotin-based stabilizer, a calcium zinc composite stabilizer or a potassium zinc composite stabilizer.
The invention also provides the flame-retardant double-layer board for space leasing, which is prepared by the preparation method of the flame-retardant double-layer board for space leasing.
In the process, the flame-retardant smoke suppressant in the flame-retardant double-layer board for space leasing does not lose flame-retardant property in the high-temperature processing process, and the generation of fragile substances is not found, so that the obtained flame-retardant double-layer board is good in mechanical property, flame-retardant and environment-friendly.
Furthermore, the flame-retardant double-layer plate for space leasing can be used for dividing space to manufacture leasing office space, and can greatly meet the requirements of the existing leasing space on flame retardance, environmental protection and durability. The flame-retardant double-layer plate for space leasing is low in cost, and the manufacturing cost of the leasing space can be indirectly reduced, so that the flame-retardant double-layer plate for space leasing has high popularization and application values.
The present invention will be described in detail below by way of examples.
Example 1
Preparing a flame-retardant double-layer plate for space leasing:
(1) preparing a flame-retardant smoke inhibitor: based on the parts by weight, 10 parts of a compound having R and represented by the formula (I)1And R2The phosphinate of the substituent, 1 part of tributyltin and 6 parts of tri-n-octylphosphine oxide are mixed for 20min at 240 ℃, and then the mixture is kept at 260 ℃ for 1.5h, wherein R1Is methyl; r2Is phenyl, M is Al, n is 3, thus obtaining the flame-retardant smoke suppressant A1;
(2) taking a first material comprising the following components in parts by weight: 75 parts of PVC-SG5 type polyvinyl chloride, 100 parts of nano calcium carbonate, 2 parts of dimethyl tin oxide PVC stabilizer, 0.5 part of stearic acid, 2 parts of ACR K-123 modifier and 115 parts of flame-retardant smoke inhibitor A; the second material includes: 75 parts of PVC-SG5 type polyvinyl chloride, 100 parts of nano calcium carbonate, 2 parts of dimethyl tin oxide PVC stabilizer, 0.5 part of stearic acid, 2 parts of ACR K-123 modifier and 110 parts of flame-retardant smoke inhibitor, respectively hot-mixing a first material and a second material at 120 ℃ for 1.5h, then cold-mixing at 60 ℃ for 20min, and then co-extruding and molding at 160 ℃. In the process, the size of the roller gap is adjusted according to the thickness required by processing, and the double-layer plate blank is co-extruded by a narrow-slit machine head after the full plasticization of a screw rod.
Example 2
Preparing a flame-retardant double-layer plate for space leasing:
(1) preparing a flame-retardant smoke inhibitor: based on the parts by weight, 10 parts of a compound having R and represented by the formula (I)1And R2Mixing the substituted phosphinate, 2 parts tributyltin and 8 parts tri-n-octylphosphine oxide at 245 ℃ for 25min, and then keeping the temperature at 270 ℃ for 2h, wherein R1Is n-propyl; r2Is isopropyl substituted by hydroxyl on 1 position, M is Al, n is 3, and the flame-retardant smoke suppressant A2 is obtained;
(2) taking a first material comprising the following components in parts by weight: 90 parts of PVC-SG5 type polyvinyl chloride, 125 parts of nano calcium carbonate, 4.5 parts of dimethyl tin oxide PVC stabilizer, 0.8 part of stearic acid, 2.8 parts of ACR K-123 modifier and 220 parts of flame-retardant smoke suppressant A; the second material includes: 95 parts of PVC-SG5 type polyvinyl chloride, 125 parts of nano calcium carbonate, 4.5 parts of dimethyl tin oxide PVC stabilizer, 0.85 part of stearic acid, 2.8 parts of ACR K-123 modifier and 211 parts of flame-retardant smoke inhibitor, respectively carrying out hot mixing on a first material and a second material at 130 ℃ for 1.2h, then carrying out cold mixing at 70 ℃ for 30min, and then carrying out extrusion molding at 180 ℃. In the process, the size of the roller gap is adjusted according to the thickness required by processing, and the double-layer plate blank is co-extruded by a narrow-slit machine head after the full plasticization of a screw rod.
Example 3
Preparing a flame-retardant double-layer plate for space leasing:
(1) preparing a flame-retardant smoke inhibitor: based on the parts by weight, 10 parts of a compound having R and represented by the formula (I)1And R2Mixing the substituted phosphinate, 3 parts of tributyltin and 10 parts of tri-n-octylphosphine oxide at 250 ℃ for 30min, and then preserving the heat at 280 ℃ for 2.5h, wherein R1Is n-hexyl substituted in position 6 by chlorine; r2Is methyl substituted by amino, M is Al, and n is 3, thus obtaining the flame-retardant smoke suppressant A3;
(2) taking a first material comprising the following components in parts by weight: 120 parts of PVC-SG5 type polyvinyl chloride, 150 parts of nano calcium carbonate, 7 parts of dimethyl tin oxide PVC stabilizer, 1.2 parts of stearic acid, 3.5 parts of ACR K-123 modifier and 325 parts of flame-retardant smoke inhibitor A; the second material includes: 120 parts of PVC-SG5 type polyvinyl chloride, 150 parts of nano calcium carbonate, 7 parts of dimethyl tin oxide PVC stabilizer, 1.2 parts of stearic acid, 3.5 parts of ACR K-123 modifier and 312 parts of flame-retardant smoke inhibitor, wherein the first material and the second material are respectively subjected to hot mixing for 2 hours at 140 ℃, then cold mixing for 40 minutes at 80 ℃, and then extrusion molding at 210 ℃. In the process, the size of the roller gap is adjusted according to the thickness required by processing, and the double-layer plate blank is co-extruded by a narrow-slit machine head after the full plasticization of a screw rod.
Example 4
Preparing a flame-retardant double-layer plate for space leasing:
(1) preparing a flame-retardant smoke inhibitor: based on the parts by weight, 10 parts of a compound having R and represented by the formula (I)1And R2Mixing the substituted phosphinate, 2 parts tributyltin and 8 parts tri-n-octylphosphine oxide at 200 ℃ for 25min, and then keeping the temperature at 200 ℃ for 2h, wherein R1Is n-propyl; r2Is isopropyl substituted by hydroxyl on 1 position, M is Al, n is 3, and the flame retardant is obtainedSmoke agent a 4;
(2) the procedure was followed as in step (2) of example 2, except that A4 was used as the flame-retardant smoke-suppressing agent.
Example 5
Preparing a flame-retardant double-layer plate for space leasing:
(1) preparing a flame-retardant smoke inhibitor: based on the parts by weight, 10 parts of a compound having R and represented by the formula (I)1And R2Mixing phosphinate of substituent groups, 2 parts of tributyltin and 8 parts of tri-n-octylphosphine oxide at 300 ℃ for 25min, and then preserving heat at 300 ℃ for 2h, wherein R1 is n-propyl; r2 is isopropyl substituted by hydroxyl on 1 position, M is Al, n is 3, and the flame-retardant smoke suppressant A5 is obtained;
(2) the procedure was followed as in step (2) of example 2, except that A5 was used as the flame-retardant smoke-suppressing agent.
Comparative example 1
A flame-retardant smoke suppressant was prepared according to the step (1) of example 2, except that the mixing temperature and the holding temperature were both 150 ℃, to obtain flame-retardant smoke suppressant B1. The flame-retardant smoke suppressant B1 was used to prepare a flame-retardant double-layer panel for space rental in accordance with the procedure (2) of example 2.
Comparative example 2
A flame-retardant smoke suppressant was prepared according to the step (1) of example 2, except that the mixing temperature and the holding temperature were both 350 ℃, to obtain flame-retardant smoke suppressant B2. The flame-retardant smoke suppressant B2 was used to prepare a flame-retardant double-layer panel for space rental in accordance with the procedure (2) of example 2.
Comparative example 3
10 parts of a compound of formula (I) having R in step (1) of example 21And R2And (3) keeping the temperature of the substituted phosphinate at 270 ℃ for 2.4h to obtain the flame-retardant smoke suppressant B3. The flame-retardant smoke suppressant B3 was used to prepare a flame-retardant double-layer panel for space rental in accordance with the procedure (2) of example 2.
Comparative example 4
10 parts of a compound of formula (I) having R in step (1) of example 21And R2The substituted phosphinate is numbered as flame retardant smoke suppressant B4. A space lease was prepared by using flame retardant and smoke suppressant B4 according to step (2) of example 2A flame retardant double layer sheet is used.
Blank control
The two-layer plate was prepared only according to the step (2) in example 2 without performing the step (1), except that the blank control polyvinyl chloride plate was obtained without adding any flame retardant and smoke suppressant.
Detection example 1
The flame-retardant double-layer plates for space renting obtained in examples 1-5 and comparative examples 1-4 are respectively correspondingly numbered as a1-a5 and b1-b4, and the tensile strength and the impact toughness of a1-a5 and b1-b4 flame-retardant polyvinyl chloride plates and blank control polyvinyl chloride plates are analyzed, wherein the detection standards are as follows: samples were prepared and tested for tensile strength according to GB/T1040.3-2006, and impact toughness was tested using GB/T1043.1-2008.
The detection shows that the trend of the tensile strength and the impact toughness of each plate is not obviously changed relative to the trend of other plates, namely the tensile strength is high and the impact toughness is also high. Among them, significant brittle fracture occurred in b3 and b4, resulting in poor tensile strength and impact toughness, with b4 being the worst, which is only 22% of the blank sample; the tensile strength and the impact toughness of the b1 and the b2 are both better than those of the b3, no obvious brittle fracture occurs, but the tensile strength and the impact toughness are different from those of the blank control sample by about 51 percent.
The order of the tensile strength and impact toughness of the other samples from good to bad was: blank control, a2, a1, a3, a4 and a5, wherein a2 is close to the blank control, and the tensile strength and the impact toughness of the blank control are more than 99 percent of those of the blank control sample; the tensile strength and the impact toughness of the a1 and the a3 are about 96 percent of those of a blank control sample; the tensile strength and the impact toughness of the a4 and the a5 are more than 88 percent of that of the blank control sample; the tensile strength of the blank control was 64 MPa.
Detection example 2
The flame-retardant double-layer plates for space renting obtained in examples 1-5 and comparative examples 1-4 are respectively correspondingly numbered as a1-a5 and b1-b4, and the oxygen index and the smoke density of a1-a5 and b1-b4 flame-retardant polyvinyl chloride plates and blank control polyvinyl chloride plates are analyzed, wherein the standard of the oxygen index test is GB/T2406.2-2009; the test standard of the smoke density is GB/T8627-2007.
The results show that the oxygen indexes of a1-a5 are all more than 27 percent and belong to flame retardants. Specifically, the oxygen indexes of a3, a2, a4, a5 and a1 are sequentially from high to low, the oxygen index of a3 reaches 43 percent, the oxygen index of a1 is 34 percent, the oxygen indexes of b1-b4 are not greatly different and are all about 29 percent, and the oxygen index of a blank control is 19 percent.
The results show that the smoke densities of a1-a5 are not very different and are all below 46SDR, the smoke densities of b1-b4 are between 48-58SDR, and the smoke density of the blank control is 68 SDR.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.
Claims (7)
1. A preparation method of a flame-retardant double-layer plate for space leasing is characterized by comprising the steps of carrying out co-extrusion molding on a first material and a second material; wherein, the first material and the second material both contain the flame-retardant smoke suppressant, wherein, the weight content of the flame-retardant smoke suppressant in the first material is 20-200% higher than that of the second material; wherein the flame-retardant smoke suppressant is prepared by reacting a compound having R as shown in formula (I)1And R2The substituted phosphinate, tributyltin and tri-n-octylphosphine oxide are prepared after heating and contacting at the temperature of 200-300 ℃;
wherein, in formula (I): r1Is C1-C6 alkyl or phenyl; r2Is C1-C6 alkyl or phenyl; m is Al, n is 3, such that Mn+Is a metal cation, wherein n + represents a charge formally assigned to the cation, and n is 3;
wherein, R is represented by the formula (I)1And R2The weight ratio of substituted phosphinate, tributyltin and tri-n-octylphosphine oxide is 10: 1-3: 8-10;
wherein, by weight, the first material comprises: 75-120 parts of polyvinyl chloride, 100 parts of filler, 150 parts of stabilizer, 0.5-1.2 parts of stearic acid, 2-3.5 parts of ACR modifier and 15-25 parts of flame-retardant smoke inhibitor; the second material includes: 75-120 parts of polyvinyl chloride, 100 parts of filler, 150 parts of stabilizer, 0.5-1.2 parts of stearic acid, 2-3.5 parts of ACR modifier and 10-12 parts of flame-retardant smoke inhibitor.
2. The method for preparing the flame-retardant double-layer board for space lease according to claim 1, wherein the temperature of heating and contacting in the preparation of the flame-retardant smoke suppressant is 240-280 ℃.
3. The method for preparing the flame-retardant double-layer board for space renting according to claim 1 or 2, wherein in the preparation of the flame-retardant smoke suppressant, the heating and contacting conditions comprise: having R as shown in formula (I)1And R2The substituted phosphinate, tributyltin and tri-n-octylphosphine oxide are mixed for 20-30min at the temperature of 240-280 ℃, and then are subjected to heat preservation for 1.5-2.5h at the temperature of 260-280 ℃.
4. The method for preparing the flame-retardant double-layer board for space renting according to claim 1 or 2, wherein the alkyl is unsubstituted or substituted by one or more of halogen, hydroxyl and amino; and/or the presence of a gas in the gas,
the phenyl is unsubstituted or substituted by one or more of halogen, hydroxyl and amino.
5. The method for preparing the flame-retardant double-layer board for space lease according to claim 1,
the first material and the second material are prepared according to the following steps: the polyvinyl chloride, the filling agent, the stabilizing agent, the stearic acid, the ACR modifier and the flame-retardant smoke suppressant are firstly hot-mixed at 140 ℃ and then cold-mixed at 60-80 ℃; and/or the presence of a gas in the gas,
the temperature of the co-extrusion molding is 160-210 ℃.
6. The method for preparing the flame-retardant double-layer board for space renting according to claim 5, wherein the polyvinyl chloride is PVC-SG5 type; and/or
The filler is one or more of heavy calcium carbonate, nano calcium carbonate, perlite, titanium dioxide and light calcium carbonate; and/or
The stabilizer is a lead salt composite stabilizer, an organic tin stabilizer, a calcium-zinc composite stabilizer or a potassium-zinc composite stabilizer.
7. A flame-retardant double-layer plate for space renting, prepared by the preparation method of any one of claims 1-6.
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| CN103030901A (en) * | 2012-12-26 | 2013-04-10 | 浙江华之杰装饰材料有限公司 | Flame-retardant and smoke-suppression PVC building template and fabrication method thereof |
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