CN113831602A - Flame-retardant celluloid board and preparation method thereof - Google Patents

Flame-retardant celluloid board and preparation method thereof Download PDF

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Publication number
CN113831602A
CN113831602A CN202111204732.9A CN202111204732A CN113831602A CN 113831602 A CN113831602 A CN 113831602A CN 202111204732 A CN202111204732 A CN 202111204732A CN 113831602 A CN113831602 A CN 113831602A
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parts
retardant
fire
solvent
mixture
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CN202111204732.9A
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徐建求
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Jiujiang Celluloid Industrial Co ltd
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Jiujiang Celluloid Industrial Co ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18Manufacture of films or sheets
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2301/00Characterised by the use of cellulose, modified cellulose or cellulose derivatives
    • C08J2301/08Cellulose derivatives
    • C08J2301/16Esters of inorganic acids
    • C08J2301/18Cellulose nitrate
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/0091Complexes with metal-heteroatom-bonds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/49Phosphorus-containing compounds
    • C08K5/51Phosphorus bound to oxygen
    • C08K5/52Phosphorus bound to oxygen only
    • C08K5/521Esters of phosphoric acids, e.g. of H3PO4
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/49Phosphorus-containing compounds
    • C08K5/51Phosphorus bound to oxygen
    • C08K5/52Phosphorus bound to oxygen only
    • C08K5/521Esters of phosphoric acids, e.g. of H3PO4
    • C08K5/523Esters of phosphoric acids, e.g. of H3PO4 with hydroxyaryl compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00Use of ingredients characterised by shape
    • C08K7/22Expanded, porous or hollow particles
    • C08K7/24Expanded, porous or hollow particles inorganic

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Fireproofing Substances (AREA)

Abstract

The invention relates to a fire-retardant celluloid board which comprises the following components in parts by weight: 65-75 parts of nitrocotton, 14-20 parts of carbon aerogel, 3-5 parts of distearoyl oxygen isopropoxy aluminate, 2-4 parts of triphenyl phosphate, 3-6 parts of a flame retardant and 60-90 parts of a solvent, wherein the carbon aerogel: distearoyl isopropoxy aluminate: triphenyl phosphate ═ 1: (4-5): (5-7). The flame retardant effect is improved through the mutual crosslinking reaction among the carbon aerogel, the distearoyl isopropoxy aluminate, the triphenyl phosphate, the flame retardant and the like. By optimizing carbon aerogels: the content of distearoyl isopropoxy aluminate and triphenyl phosphate further increases the tensile strength.

Description

Flame-retardant celluloid board and preparation method thereof
Technical Field
The invention relates to the technical field of celluloid boards, in particular to a component of a flame-retardant celluloid board and a preparation method thereof.
Background
The celluloid board as a plastic product developed and used earlier by human beings has better water resistance, acid resistance and oil resistance, and is widely applied to daily life of people. However, the celluloid board has a fatal defect, and is easy to burn, so that the use of the celluloid board in large quantity has potential safety hazard. In order to overcome the flammability of the celluloid board, a flame retardant is often added to the components of the celluloid board, but the flame retardant effect of the existing flame retardant is not obvious, and other properties of the celluloid board are also affected to a certain extent. Therefore, there is a need to improve the composition of celluloid board to improve its performance.
Disclosure of Invention
Aiming at the technical problem that the flame retardant effect of the celluloid board prepared by using the conventional common flame retardant is not obvious, the invention improves the flame retardant property of the celluloid board and enhances the tensile property of the celluloid board by optimizing the component design and using the components such as carbon aerogel, distearoyl isopropoxy aluminate and triphenyl phosphate.
In order to achieve the purpose, the invention adopts the following technical scheme:
a flame-retardant celluloid board, which comprises the following components in parts by weight: 65-75 parts of nitrocotton, 14-20 parts of carbon aerogel, 3-5 parts of distearoyl oxygen isopropoxy aluminate, 2-4 parts of triphenyl phosphate, 3-6 parts of a flame retardant and 60-90 parts of a solvent, wherein the carbon aerogel: distearoyl isopropoxy aluminate: triphenyl phosphate ═ 1: (4-5): (5-7).
Specifically, the flame-retardant celluloid board comprises 68-72 parts of nitrocotton, 16-18 parts of carbon aerogel, 3-5 parts of distearoyl isopropoxy aluminate, 2-4 parts of triphenyl phosphate, 3-5 parts of a flame retardant and 75-90 parts of a solvent.
Specifically, the flame-retardant celluloid board comprises 70 parts of nitrocotton, 16 parts of carbon aerogel, 4 parts of distearoyl oxy isopropoxy aluminate, 3 parts of triphenyl phosphate, 5 parts of a flame retardant and 80 parts of a solvent.
Specifically, the flame retardant is trihaloethyl phosphate or tri (trihalophenyl) phosphate.
Specifically, the solvent is a mixture of any two of ethanol, propanol, acetone and butanone.
A preparation method of flame-retardant celluloid board comprises the following steps:
(1) adding nitrocotton and a flame retardant into a solvent, and stirring and mixing to obtain a mixture A;
(2) mixing and stirring carbon aerogel, distearoyl isopropoxy aluminate and triphenyl phosphate in a solvent, and standing for a period of time to obtain a mixture B; reacting and crosslinking the carbon aerogel, distearoyl isopropoxy aluminate and triphenyl phosphate;
(3) stirring, mixing and standing the mixture A and the mixture B for a period of time, and performing filter pressing treatment to obtain a mixture C;
(4) plasticizing and calendering the mixture C.
Specifically, the solvent is at least one of ethanol, propanol, acetone and butanone.
Specifically, in the step (1), the weight ratio of the solvent to the nitrocotton is 0.8-1, and the weight ratio can be 0.8, 0.9 or 1.
Specifically, in the step (2) and the step (3), the standing time is 0.5-1h, and can be 0.5h, 0.7h or 1 h.
Specifically, in the step (4), the plasticizing temperature is 80-150 ℃, and can be 80 ℃, 100 ℃, 110 ℃, 120 ℃, 130 ℃ or 150 ℃, and the calendering temperature is 90-110 ℃, and can be 90 ℃, 100 ℃ or 110 ℃.
The celluloid board disclosed by the invention has the advantage that the flame retardant effect is improved by adding the carbon aerogel, the distearoyl isopropoxy aluminate, the triphenyl phosphate, the flame retardant and the like through the mutual crosslinking reaction among the components. By optimizing carbon aerogels: the content of distearoyl isopropoxy aluminate and triphenyl phosphate further increases the tensile strength.
Detailed Description
The following detailed description of embodiments of the invention, but the invention can be practiced in many different ways, as defined and covered by the claims.
Table 1: content of each component of celluloid board (parts by weight)
Figure BDA0003306394520000031
Among them, the flame retardants of examples 1 to 3 and comparative examples 1 to 2 were selected from trihaloethyl phosphate, and the flame retardants of examples 4 to 5 and comparative example 3 were selected from tris (trihalophenyl) phosphate.
Examples 1-5 and comparative examples 1-3 were prepared as follows:
a preparation method of flame-retardant celluloid board is characterized by comprising the following steps:
(1) adding nitrocotton and a flame retardant into a part of solvent, stirring and mixing to obtain a mixture A, wherein the weight ratio of the solvent to the nitrocotton is 0.8;
(2) mixing and stirring carbon aerogel, distearoyl isopropoxy aluminate and triphenyl phosphate in the rest part of solvent, and standing for 0.5h to obtain a mixture B;
(3) stirring, mixing and standing the mixture A and the mixture B for 0.5h, and performing filter pressing treatment to obtain a mixture C;
(4) plasticizing the mixture C at 100 ℃, calendering the mixture C at 110 ℃, and cooling the mixture C to prepare the flame-retardant celluloid board.
The fire-retardant celluloid boards prepared in examples 1-5 and comparative examples 1-3 were subjected to fire-retardant test (refer to UL94 fire-retardant test standard) and tensile strength test (GB/T1040.2-2006), and the average results of the three tests are shown in the following table:
TABLE 2 flame retardant rating and tensile strength of the flame retardant celluloid boards prepared in examples 1-5 and comparative examples 1-3
Flame retardant rating Tensile Strength (MPa)
Example 1 V-1 65.6
Example 2 V-1 66.2
Example 3 V-1 65.3
Example 4 V-2 67.1
Example 5 V-1 65.4
Comparative example 1 V-0 55.4
Comparative example 2 HB 47.6
Comparative example 3 Is free of 46.3
As can be seen from the test results of Table 2, the flame retardant properties and tensile strength of examples 1 to 5 are significantly superior to those of comparative examples 2 to 3.
This is because the flame retardant effect is enhanced by the mutual crosslinking reaction among the carbon aerogel, distearoyl isopropoxy aluminate, triphenyl phosphate, the flame retardant, and the like. By optimizing carbon aerogels: the content of distearoyl isopropoxy aluminate and triphenyl phosphate further increases the tensile strength.
The above description is only a preferred embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, which are made by the present specification, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.

Claims (10)

1. A flame-retardant celluloid board, which is characterized by comprising the following components in parts by weight: 65-75 parts of nitrocotton, 14-20 parts of carbon aerogel, 3-5 parts of distearoyl oxygen isopropoxy aluminate, 2-4 parts of triphenyl phosphate, 3-6 parts of a flame retardant and 60-90 parts of a solvent, wherein the carbon aerogel: distearoyl isopropoxy aluminate: triphenyl phosphate ═ 1: (4-5): (5-7).
2. The fire-retardant celluloid board according to claim 1, comprising 68-72 parts of nitrocotton, 16-18 parts of carbon aerogel, 3-5 parts of distearoyl isopropoxy aluminate, 2-4 parts of triphenyl phosphate, 3-5 parts of fire retardant and 75-90 parts of solvent.
3. The fire-retardant celluloid board according to claim 1, comprising 70 parts of nitrocotton, 16 parts of carbon aerogel, 4 parts of distearoyl isopropoxy aluminate, 3 parts of triphenyl phosphate, 5 parts of fire retardant and 80 parts of solvent.
4. The fire-resistant celluloid board according to claim 1, wherein the fire retardant is trihaloethyl phosphate or tris (trihalophenyl) phosphate.
5. The fire-retardant celluloid board according to claim 1, wherein the solvent is a mixture of any two of ethanol, propanol, acetone and butanone.
6. A preparation method of flame-retardant celluloid board is characterized by comprising the following steps:
(1) adding nitrocotton and a flame retardant into a solvent, and stirring and mixing to obtain a mixture A;
(2) mixing and stirring carbon aerogel, distearoyl isopropoxy aluminate and triphenyl phosphate in a solvent, and standing for a period of time to obtain a mixture B;
(3) stirring, mixing and standing the mixture A and the mixture B for a period of time, and performing filter pressing treatment to obtain a mixture C;
(4) plasticizing and calendering the mixture C.
7. The method for preparing fire-retardant celluloid board according to claim 6, wherein the solvent is at least one of ethanol, propanol, acetone and butanone.
8. The method for preparing a fire-retardant celluloid board according to claim 6, wherein in step (1), the weight ratio of the solvent to the nitrocotton is 0.8-1.
9. The method for preparing a fire-retardant celluloid board according to claim 6, wherein the standing time in step (2) and step (3) is 0.5-1 h.
10. The method for preparing a fire-retardant celluloid board according to claim 6, wherein in the step (4), the plasticizing temperature is 80-150 ℃ and the rolling temperature is 90-110 ℃.
CN202111204732.9A 2021-10-15 2021-10-15 Flame-retardant celluloid board and preparation method thereof Pending CN113831602A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4764539A (en) * 1987-11-24 1988-08-16 Norton Company Flame resistant polymers
CN104558691A (en) * 2013-10-14 2015-04-29 刘新智 Nitrocotton for flame-retardant celluloid and preparation method of nitrocotton product
CN106279775A (en) * 2015-05-18 2017-01-04 刘新智 Flame retardancy celluloid raw material, sheet material bar and the preparation method of industrial products thereof
CN106928908A (en) * 2017-02-19 2017-07-07 广州市芯检康生物科技有限公司 A kind of new aeroge multifunctional material and preparation method thereof
US20190352473A1 (en) * 2018-05-17 2019-11-21 Niching Industrial Corp. Flame-retardant and abrasion-resistant composite
US10711070B1 (en) * 2017-03-22 2020-07-14 The United States Of America As Represented By The Secretary Of The Army Method for preparing spherical celluloid beads

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4764539A (en) * 1987-11-24 1988-08-16 Norton Company Flame resistant polymers
CN104558691A (en) * 2013-10-14 2015-04-29 刘新智 Nitrocotton for flame-retardant celluloid and preparation method of nitrocotton product
CN106279775A (en) * 2015-05-18 2017-01-04 刘新智 Flame retardancy celluloid raw material, sheet material bar and the preparation method of industrial products thereof
CN106928908A (en) * 2017-02-19 2017-07-07 广州市芯检康生物科技有限公司 A kind of new aeroge multifunctional material and preparation method thereof
US10711070B1 (en) * 2017-03-22 2020-07-14 The United States Of America As Represented By The Secretary Of The Army Method for preparing spherical celluloid beads
US20190352473A1 (en) * 2018-05-17 2019-11-21 Niching Industrial Corp. Flame-retardant and abrasion-resistant composite

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
刘玉荣 著: "《碳材料在超级电容器中的应用》", 31 January 2013, 国防工业出版社 *

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