CN107915917B - Flame-retardant three-layer plate for space leasing and preparation method thereof - Google Patents

Flame-retardant three-layer plate for space leasing and preparation method thereof Download PDF

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CN107915917B
CN107915917B CN201710982223.6A CN201710982223A CN107915917B CN 107915917 B CN107915917 B CN 107915917B CN 201710982223 A CN201710982223 A CN 201710982223A CN 107915917 B CN107915917 B CN 107915917B
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flame
layer
retardant
parts
flame retardant
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CN107915917A (en
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刘傲
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Anhui Yiheng Yunchuang Technology Co ltd
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Anhui Yiheng Information Technology Co Ltd
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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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B32B27/08—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/18—Layered products comprising a layer of synthetic resin characterised by the use of special additives
    • B32B27/20—Layered products comprising a layer of synthetic resin characterised by the use of special additives using fillers, pigments, thixotroping agents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/30—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers
    • B32B27/304—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers comprising vinyl halide (co)polymers, e.g. PVC, PVDC, PVF, PVDF
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/30—Properties of the layers or laminate having particular thermal properties
    • B32B2307/306—Resistant to heat
    • B32B2307/3065—Flame resistant or retardant, fire resistant or retardant
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2419/00—Buildings or parts thereof
    • 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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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Laminated Bodies (AREA)

Abstract

The invention discloses a flame-retardant three-layer plate for space leasing and a preparation method thereof, wherein the flame-retardant three-layer plate comprises the following steps: respectively mixing the first layer of material, the second layer of material and the third layer of material, and then co-extruding and molding; wherein, the materials comprise flame retardant, and the weight content of the flame retardant in the first layer material and the third layer material is 20-200% higher than that of the second layer material; wherein the flame retardant is prepared by reacting a compound represented by the formula (I) having R1And R2The substituted phosphinate, tributyltin, tri-n-octylphosphine oxide and melamine are heated and contacted at the temperature of 220-280 ℃ to prepare the compound. The flame retardant in the plate does not lose flame retardant property in the high-temperature processing process, and the generation of brittle substances is not found, so that the plate is good in mechanical property, flame retardant and environment-friendly. The flame-retardant three-layer plate for space leasing has lower cost, and can indirectly reduce the manufacturing cost of the leasing space, thereby having very high popularization and application values.

Description

Flame-retardant three-layer plate for space leasing and preparation method thereof
Technical Field
The invention relates to a flame-retardant plate, in particular to a flame-retardant three-layer plate 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 retardants include aluminum hydroxide, cerium hydroxide, magnesium hydroxide, halogen flame retardants, phosphinates, and polycyanulars, and although halogen flame retardants commonly used at present are 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, patent document US2007/0029532 discloses that phosphonates may cause decomposition during processing and generate brittle unusable substances during processing, thus limiting the use of phosphonates as flame retardants.
Patent document CN107207779A, entitled: flame retardant polymer compositions comprising heat treated phosphorus compounds and melam disclose that flame retardants 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 incorporating into the polymer. However, the melam or melam derivatives are not easily synthesized, which increases the application cost of the flame retardant containing melam.
Therefore, it is an urgent technical problem to solve how to provide a flame retardant and a board containing the flame retardant, which can reduce the production cost of the material, improve the flame retardant performance of the material in application, generate no fragile substances, and 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 three-layer board for space leasing contains a flame retardant, and the flame retardant can improve the flame retardant performance of the flame-retardant three-layer board in application materials on the basis of keeping the advantages of low smoke density of phosphinate, no environmental hazard and the like, does not generate fragile substances, does not reduce the influence on the mechanical properties of main material matrixes, and is more economical in used auxiliaries.
In order to realize the purpose, the invention provides a preparation method of a flame-retardant three-layer plate for space leasing, which comprises the following steps: respectively mixing the first layer of material, the second layer of material and the third layer of material, and then co-extruding and molding; wherein, the first layer material, the second layer material and the third layer material all comprise flame retardant, and the weight content of the flame retardant in the first layer material and the third layer material is 20-200% higher than that of the second layer material; wherein the flame retardant is prepared by reacting a compound represented by the formula (I) having R1And R2The substituted phosphinate, tributyltin, tri-n-octylphosphine oxide and melamine are heated and contacted at the temperature of 220-280 ℃ to prepare the compound; wherein, in formula (I): r1Is C1-C6 alkyl or phenyl; r2Is C1-C6 alkyl or phenyl; m is a metal element, and n is a positive integer from 1 to 4.
Figure DEST_PATH_IMAGE001
The invention also provides the flame-retardant three-layer plate for space leasing, which is prepared by the preparation method of the flame-retardant three-layer plate for space leasing.
The flame retardant in the flame-retardant three-layer plate for space leasing does not lose flame-retardant performance in the high-temperature processing process, and the generation of fragile substances is not found, so that the obtained flame-retardant three-layer plate is good in mechanical performance, flame-retardant and environment-friendly. The flame-retardant three-layer plate for space leasing is formed by co-extruding the first layer material, the second layer material and the third layer material, so that the strength of the material is higher, and the weight content of the flame retardant in the first layer material and the third layer material is 20-200% higher than that of the second layer material, so that the raw material cost can be reduced on the basis of ensuring flame retardance. The flame-retardant three-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 three-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 three-layer plate 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, which is prepared by mixing a compound shown as a formula (I) and provided with R1And R2The substituted phosphinate, tributyltin, tri-n-octylphosphine oxide and melamine are heated and contacted at the temperature of 220-280 ℃ to prepare the compound; wherein, in formula (I): r1Is C1-C6 alkyl or phenyl; r2Is C1-C6 alkyl or phenyl; m is a metal element, and n is a positive integer from 1 to 4.
Figure 162518DEST_PATH_IMAGE001
According to the technical scheme, the flame retardant can be obtained by a person skilled in the art by selecting the raw material types and the preparation process. The flame retardant 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 can be improved by melamine. The preparation raw materials of the flame retardant are cheap and easy to obtain, so that the flame retardant 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 of the present invention can be added to various raw materials for preparing polymers such as plastics or rubbers to obtain target materials for improving 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 oxides, styrene polymers and copolymers, polycarbonates, acrylic polymers, polyamides, polyacetals, epoxy resins are main matrices.
In this process, the flame retardant of the present 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 of the present invention to a material mainly composed of polyvinyl chloride will be described.
In the present invention, in order to obtain a flame retardant 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 material with excellent flame retardant property after processingThe flame retardant has less fragile substances and good mechanical properties of the processed material, and more preferably, the heating contact conditions comprise: having R as shown in formula (I)1And R2The phosphinate of substituent groups, tributyltin and tri-n-octylphosphine oxide are mixed for 20-30min at the temperature of 240-250 ℃, then are insulated for 1.5-2.5h at the temperature of 260-280 ℃, and are mixed for 30-40min by adding melamine at the temperature of 240-260 ℃. 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 R2The weight ratio of substituted phosphinates, tributyltin, tri-n-octylphosphine oxide and melamine can be adjusted within a wide range, and the flame retardant in the application can be obtained. In order to obtain a flame retardant with excellent flame retardant property, less fragile substances in the processed material and good mechanical property of the processed material, the flame retardant with R shown in formula (I)1And R2The weight ratio of substituted phosphinate, tributyltin, tri-n-octylphosphine oxide and melamine is 10: 1-3: 8-10: 2-4.
The invention also provides a flame retardant prepared according to the preparation method of the flame retardant.
Through the technical scheme, the flame retardant 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 substrate. The preparation raw materials of the flame retardant are cheap and easy to obtain, so that the flame retardant has higher popularization and application values.
The invention also provides a preparation method of the flame-retardant three-layer plate for space leasing, which comprises the following steps: respectively mixing the first layer of material, the second layer of material and the third layer of material, and then co-extruding and molding; wherein, the first layer material, the second layer material and the third layer material all comprise flame retardant, and the weight content of the flame retardant in the first layer material and the third layer material is 20-200% higher than that of the second layer material; wherein the flame retardant is the flame retardant provided by the invention and described above.
In the process, the flame retardant in the flame-retardant three-layer plate for space leasing does not lose the flame-retardant property in the high-temperature processing process, and the generation of fragile substances is not found, so that the obtained flame-retardant three-layer plate is a flame-retardant material with good mechanical property, flame retardance and environmental protection. The flame-retardant three-layer plate for space leasing is formed by co-extruding the first layer material, the second layer material and the third layer material, so that the strength of the material is higher, and the weight content of the flame retardant in the first layer material and the third layer material is 20-200% higher than that of the second layer material, so that the raw material cost can be reduced on the basis of ensuring flame retardance.
Aiming at the current situation, the flame-retardant three-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 three-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 three-layer plate has high popularization and application values.
The raw materials in the flame-retardant three-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 layer of material comprises the following components in parts by weight: 75-120 parts of polyvinyl chloride, 100-150 parts of filler, 2-7 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; the second layer material comprises 95-130 parts of polyvinyl chloride, 150 parts of filler 100-; the third layer material comprises 75-120 parts of polyvinyl chloride, 100 parts of filler and 150 parts of stabilizer, 2-7 parts of stearic acid, 0.5-1.2 parts of ACR modifier and 15-25 parts of flame retardant.
The mixing conditions of the first layer material, the second layer material and the third layer material can be adjusted within a wide range by those skilled in the art, and in order to obtain a plate with good mechanical properties and flame retardance, the mixing conditions of the first layer material, the second layer material and the third layer material are preferably as follows: firstly, hot mixing at the temperature of 120 ℃ and 140 ℃, and then cold mixing at the temperature of 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.
The coextrusion conditions can be adjusted within a wide range by those skilled in the art, and the temperature of the coextrusion molding is preferably 160-210 ℃.
And adjusting the size of the roller gap according to the thickness required by processing. After being fully plasticized by the screw rod, the three-layer plate blank is extruded by a narrow-seam 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 three-layer plate for space leasing, which is prepared by the preparation method of the flame-retardant three-layer plate for space leasing.
In the process, the flame retardant in the flame-retardant three-layer plate for space leasing does not lose the flame-retardant property in the high-temperature processing process, and the generation of fragile substances is not found, so that the obtained flame-retardant three-layer plate is good in mechanical property, flame-retardant and environment-friendly. The flame-retardant three-layer plate for space leasing is formed by co-extruding the first layer material, the second layer material and the third layer material, so that the strength of the material is higher, and the weight content of the flame retardant in the first layer material and the third layer material is 20-200% higher than that of the second layer material, so that the raw material cost can be reduced on the basis of ensuring flame retardance.
Furthermore, the flame-retardant three-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 three-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 three-layer plate has high popularization and application values.
The present invention will be described in detail below by way of examples.
Example 1
The preparation method of the flame-retardant three-layer plate for space leasing comprises the following steps:
(1) preparing a flame retardant: 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, 1 part of tributyltin and 8 parts of tri-n-octylphosphine oxide at 220 ℃ for 20min, then preserving heat at 260 ℃ for 1.5h, adding 2 parts of melamine at 240 ℃ and mixing for 30min, wherein R1 is methyl; r2 is phenyl, M is Al, n is 3, and a flame retardant A1 is obtained;
(2) the first layer of material comprises 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 A; the first layer of material comprises: 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 A; the third layer of material comprises 75 parts of polyvinyl chloride, 100 parts of filler, 2 parts of stabilizer, 0.5 part of stearic acid, 2 parts of ACR modifier and 115 parts of flame retardant A; respectively hot-mixing at 120 deg.C for 1.5 hr, cold-mixing at 60 deg.C for 20min, and extruding at 160 deg.C. And adjusting the size of the roller gap according to the thickness required by processing. After being fully plasticized by the screw rod, the three-layer plate blank is extruded by a narrow-seam 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.
Figure 242469DEST_PATH_IMAGE001
Example 2
The preparation method of the flame-retardant three-layer plate for space leasing comprises the following steps:
(1) preparing a flame retardant: 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 9 parts of tri-n-octylphosphine oxide at 245 ℃ for 25min, then preserving heat at 270 ℃ for 1.5h, adding 3 parts of melamine at 250 ℃ and mixing for 35min, wherein R1 is n-propyl; r2 is isopropyl substituted by hydroxyl at position 1, M is Al, n is 3, and flame retardant A2 is obtained;
(2) the first layer of material comprises 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, 0.85 part of stearic acid, 2.2 parts of ACR K-123 modifier and 120 parts of flame retardant A; the first layer of material comprises: 90 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, 2.2 parts of ACR K-123 modifier and 111 parts of flame retardant A; the third layer material comprises 90 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, 2.2 parts of ACR K-123 modifier and 120 parts of flame retardant A. Respectively hot-mixing at 130 deg.C for 1.6 hr, cold-mixing at 70 deg.C for 30min, and extruding at 185 deg.C. And adjusting the size of the roller gap according to the thickness required by processing. After being fully plasticized by the screw rod, the three-layer plate blank is extruded by a narrow-seam 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.
Example 3
The preparation method of the flame-retardant three-layer plate for space leasing comprises the following steps:
(1) preparing a flame retardant: 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, 1-3 parts of tributyltin and 8-10 parts of tri-n-octylphosphine oxide at 250 ℃ for 30min, then preserving heat at 280 ℃ for 2.5h, adding 4 parts of melamine at 260 ℃ and mixing for 40min, wherein R1 is n-hexyl substituted by chlorine at the 6-position; r2 is substituted by aminoMethyl, M is Al, n is 3, and a flame retardant A3 is obtained;
(2) the first layer of material comprises 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 125 parts of flame retardant A; the first layer of material comprises: 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 112 parts of flame retardant A; the third layer material comprises 120 parts of polyvinyl chloride, 150 parts of filler, 7 parts of stabilizer, 1.2 parts of stearic acid, 3.5 parts of ACR modifier and 125 parts of flame retardant A. Respectively hot-mixing at 140 deg.C for 2 hr, cold-mixing at 80 deg.C for 40min, and extruding at 210 deg.C. And adjusting the size of the roller gap according to the thickness required by processing. After being fully plasticized by the screw rod, the three-layer plate blank is extruded by a narrow-seam 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.
Comparative example 1
A flame retardant was prepared by following the procedure (1) of example 2, except that the mixing temperature and the holding temperature were both 150 ℃ to obtain flame retardant B1. Flame retardant B1 flame retardant three-layer board for space renting was prepared according to the step (2) in example 2.
Comparative example 2
A flame retardant was prepared by following the procedure (1) of example 2, except that the mixing temperature and the holding temperature were both 350 ℃ to obtain flame retardant B2. Flame retardant B2 flame retardant three-layer board for space renting was prepared according to the step (2) in example 2.
Comparative example 3
Example 210 parts of a compound of formula (I) having R1And R2And (3) keeping the temperature of the substituted phosphinate at 270 ℃ for 2.4h to obtain the flame retardant B3. Flame retardant B3 flame retardant three-layer board for space renting was prepared according to the step (2) in example 2.
Comparative example 4
Example 210 parts of a compound of formula (I) having R1And R2The substituted phosphinate was numbered flame retardant B4. Will be provided withFlame retardant B4A flame retardant three-layer panel for space renting was prepared according to the procedure (2) in example 2.
Blank control
A flame-retardant three-layer plate for space renting was prepared according to the step (2) in example 2, except that no flame retardant was added.
Detection example 1
The flame-retardant three-layer plates for space renting obtained in examples 1-3 and comparative examples 1-4 are respectively correspondingly numbered as a1-a3 and b1-b4, and the tensile strength and the impact toughness of the a1-a3 and b1-b4 and a blank control polyvinyl chloride plate are detected according to the detection standards: 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, only 20% of the blank; 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 52 percent.
The order of the tensile strength and impact toughness of the other samples from good to bad was: blank control, a2, a1 and a3, wherein the a2 is close to the blank control, and the tensile strength and the impact toughness are more than 97 percent of the blank control sample; the tensile strength and the impact toughness of the a1 and the a3 are about 94 percent of those of the blank control sample; the tensile strength of the blank control was 62 MPa.
Detection example 2
The flame-retardant three-layer plates for space renting obtained in examples 1-3 and comparative examples 1-4 are respectively correspondingly numbered as a1-a3 and b1-b4, and the oxygen index and the smoke density of a1-a3 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-a3 are all more than 27 percent and belong to flame retardants. Specifically, the oxygen indexes are a3, a2 and a1 from high to low, the oxygen index of a3 reaches 43 percent, the oxygen index of a1 is 36 percent, the oxygen indexes of b1-b4 are not greatly different and are all around 30 percent, and the oxygen index of a blank control is 18 percent.
The results show that the smoke densities of a1-a3 are not very different and are all below 45SDR, the smoke densities of b1-b4 are between 49 and 58SDR, and the smoke density of the blank control is 67 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 three-layer plate for space leasing is characterized by comprising the following steps: respectively mixing the first layer of material, the second layer of material and the third layer of material, and then co-extruding and molding; wherein, the first layer material, the second layer material and the third layer material all comprise flame retardant, and the weight content of the flame retardant in the first layer material and the third layer material is 20-200% higher than that of the second layer material;
wherein the flame retardant is prepared by reacting a compound represented by the formula (I) having R1And R2The substituted phosphinate, tributyltin, tri-n-octylphosphine oxide and melamine are heated and contacted at the temperature of 220-280 ℃ to prepare the compound;
Figure 194585DEST_PATH_IMAGE001
wherein, in formula (I): r1Is C1-C6 alkyl or phenyl; r2Is C1-C6 alkyl or phenyl; m is Al, n is 3;
wherein the alkylphosphinic acid salt of formula (I) has R1And R2The weight ratio of substituted phosphinate, tributyltin, tri-n-octylphosphine oxide and melamine is 10: 1-3: 8-10: 2-4;
wherein, by weight, the first layer of material comprises: 75-120 parts of polyvinyl chloride, 100-150 parts of filler, 2-7 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; the second layer material comprises 95-130 parts of polyvinyl chloride, 150 parts of filler 100-; the third layer material comprises 75-120 parts of polyvinyl chloride, 100 parts of filler and 150 parts of stabilizer, 2-7 parts of stearic acid, 0.5-1.2 parts of ACR modifier and 15-25 parts of flame retardant.
2. The method for preparing the flame-retardant three-layer plate for space renting as claimed in claim 1, wherein the temperature of heating contact in the preparation of the flame retardant is 240-280 ℃.
3. The preparation method of the flame-retardant three-layer plate for space renting according to claim 1 or 2, wherein in the preparation of the flame retardant, the heating and contacting conditions comprise: having R as shown in formula (I)1And R2The phosphinate of substituent groups, tributyltin and tri-n-octylphosphine oxide are mixed for 20-30min at the temperature of 240-250 ℃, then are insulated for 1.5-2.5h at the temperature of 260-280 ℃, and are mixed for 30-40min by adding melamine at the temperature of 240-260 ℃.
4. The preparation method of the flame-retardant three-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 preparation method of the flame-retardant three-layer board for space renting according to claim 1, wherein the mixing conditions of the first layer material, the second layer material and the third layer material are respectively as follows: firstly, hot mixing at the temperature of 120-140 ℃, and then cold mixing at the temperature of 60-80 ℃; and/or the temperature of the co-extrusion molding is 160-210 ℃.
6. The method for preparing a flame-retardant three-layer plate 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 presence of a gas in the gas,
the stabilizer is a lead salt composite stabilizer, an organic tin stabilizer, a calcium-zinc composite stabilizer or a potassium-zinc composite stabilizer.
7. The flame-retardant three-layer board for space renting, prepared by the preparation method of the flame-retardant three-layer board for space renting as set forth in any one of claims 1-6.
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