CN113234254A - Intercalated hydrotalcite flame-retardant smoke suppressant and preparation method thereof - Google Patents
Intercalated hydrotalcite flame-retardant smoke suppressant and preparation method thereof Download PDFInfo
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- CN113234254A CN113234254A CN202110460063.5A CN202110460063A CN113234254A CN 113234254 A CN113234254 A CN 113234254A CN 202110460063 A CN202110460063 A CN 202110460063A CN 113234254 A CN113234254 A CN 113234254A
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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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
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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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
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/34—Heterocyclic compounds having nitrogen in the ring
- C08K5/3467—Heterocyclic compounds having nitrogen in the ring having more than two nitrogen atoms in the ring
- C08K5/3477—Six-membered rings
- C08K5/3492—Triazines
- C08K5/34928—Salts
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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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/22—Halogen free composition
Abstract
The invention discloses an insertion-layer type hydrotalcite flame-retardant smoke suppressant and a preparation method thereof, wherein the preparation method of the insertion-layer type hydrotalcite flame-retardant smoke suppressant comprises the following steps: the hydrotalcite is uniformly dispersed in a water phase, ultrasonically dispersed for 30 minutes, added with dodecyl sulfopropyl betaine, stirred and reacted at a certain temperature, separated to prepare the dodecyl sulfopropyl betaine surface organic treatment hydrotalcite, added with the dodecyl sulfopropyl betaine surface organic treatment hydrotalcite into distilled water, ultrasonically dispersed, dropwise added with a solution containing melamine polyphosphate/hydrochloric acid, the pH value of which is 3.0-5.0, stirred and reacted at 25-60 ℃ for 2-8 hours to obtain a suspension, the suspension obtained by the reaction is filtered, washed with distilled water for multiple times and dried in a drying oven at 100 ℃ for 24 hours to prepare the intercalation type hydrotalcite flame-retardant smoke suppressant.
Description
Technical Field
The invention relates to the technical field of flame retardants, in particular to an insertion-type hydrotalcite flame-retardant smoke suppressant and a preparation method thereof.
Background
With the progress of science and technology, the production and living standards of people are continuously improved, and various high polymer materials are more and more widely applied and play an important role in national economy. Most of the high molecular materials are flammable and release a large amount of smoke and toxic substances during combustion. The existing research shows that more than 90% of deaths in fire are caused by the inhalation of smoke dust and toxic gas, so that the problem of smoke suppression in the combustion of high polymer materials is one of the key problems in the flame retardant field. Hydrotalcite has the advantages of low toxicity, no corrosion, low cost, wide source and the like, and is considered to be the flame-retardant smoke suppressant with the most development prospect. However, hydrotalcite has the disadvantages of easy agglomeration, poor compatibility with polymers and the like, and needs to be organically modified, and commonly used modifiers comprise organic acids, various surfactants and coupling agents. Although the mechanical property of the matrix material is improved by the common modifier, the flame-retardant and smoke-suppression efficiency of the hydrotalcite is reduced, and the aims of high-efficiency flame-retardant and smoke-suppression and effective enhancement and modification of the flame retardant are difficult to realize.
The molecular structure design is carried out based on the synergistic flame retardance, the self-enhancement and the nano effect, the intercalation type hydrotalcite flame-retardant smoke suppressant is prepared by utilizing an ion exchange reaction intercalation method, the synchronous improvement of the synergistic flame retardance, the smoke suppression and the self-enhancement of the functionalized hydrotalcite is realized, the multiple modification purposes of flame retardance, smoke suppression and enhancement of a high-molecular elastomer material are achieved, and the technical problems of low flame-retardant smoke suppressant efficiency and poor enhancement modification effect of hydroxide smoke suppressants are solved. The intercalation type hydrotalcite flame-retardant smoke suppressant is a halogen-free flame retardant and has the advantages of environmental protection; the flame retardant effect of the polymer can be improved by using the synergistic flame retardant of the intumescent flame retardant and the hydrotalcite; the dosage of the flame retardant in the polymer is reduced, and the production cost of the flame-retardant material can be reduced to the maximum extent. Therefore, the intercalated hydrotalcite flame-retardant smoke suppressant provides a new approach for preparing a high-efficiency, low-cost, low-toxicity, low-smoke and environment-friendly flame-retardant polymer material.
Disclosure of Invention
This section is for the purpose of summarizing some aspects of embodiments of the invention and to briefly introduce some preferred embodiments. In this section, as well as in the abstract and the title of the invention of this application, simplifications or omissions may be made to avoid obscuring the purpose of the section, the abstract and the title, and such simplifications or omissions are not intended to limit the scope of the invention.
The present invention has been made in view of the above and/or problems occurring in the conventional flame retardants.
Therefore, the invention aims to provide the intercalated hydrotalcite flame-retardant smoke suppressant which does not contain halogen, has good flame-retardant and smoke-suppressant effects and wide application range and meets the requirement of environmental protection.
To solve the above technical problem, according to an aspect of the present invention, the present invention provides the following technical solutions:
an insertion-layer type hydrotalcite flame-retardant smoke suppressant comprises the following components in parts by mass:
1000g of distilled water, 100g of hydrotalcite, 6-20 g of dodecyl sulfopropyl betaine and 3-15 g of melamine polyphosphate.
As a preferable scheme of the intercalated hydrotalcite flame-retardant smoke suppressant, the intercalated hydrotalcite flame-retardant smoke suppressant comprises 1000g of distilled water, 100g of hydrotalcite, 20g of dodecyl sulfopropyl betaine and 15g of melamine polyphosphate according to the mass part ratio.
A preparation method of an intercalation type hydrotalcite flame-retardant smoke suppressant comprises the following specific steps:
s1, uniformly dispersing hydrotalcite in a water phase, performing ultrasonic dispersion for 30 minutes, adding dodecyl sulfopropyl betaine, stirring and reacting for 4-15 hours at the temperature of 60-90 ℃, and separating to obtain the dodecyl sulfopropyl betaine surface organic treatment hydrotalcite;
s2, adding the organic surface treatment hydrotalcite of dodecyl sulfopropyl betaine into 1000g of distilled water, ultrasonically dispersing for 30 minutes, transferring into a three-neck flask provided with a mechanical stirrer, a thermometer and a reflux condenser tube, dropwise adding a melamine polyphosphate/hydrochloric acid solution with the pH value of 3.0-5.0, and stirring at 25-60 ℃ for reaction for 2-8 hours to obtain a suspension;
s3, filtering the suspension obtained by the reaction, washing the suspension for multiple times by using distilled water, and drying the suspension in an oven at 100 ℃ for 24 hours to obtain the intercalated hydrotalcite flame-retardant smoke suppressant.
As a preferable embodiment of the preparation method of the intercalated hydrotalcite flame-retardant smoke suppressant of the present invention, in step S1, the product obtained by filtration is washed with distilled water for a plurality of times, and the obtained solid is dried by forced air to a constant weight to obtain the dodecylsulfopropyl betaine surface organically treated hydrotalcite.
As a preferable embodiment of the method for preparing an intercalated hydrotalcite flame retardant and smoke suppressant according to the present invention, in step S3, the suspension obtained by the reaction is filtered and washed three times with distilled water.
Compared with the prior art, the invention has the beneficial effects that: the intercalated hydrotalcite flame-retardant smoke suppressant adopts a halogen-free flame-retardant system, utilizes the synergistic flame-retardant effect of the melamine polyphosphate and the hydrotalcite, improves the flame-retardant and smoke-suppressant effects on the polymer, reduces the use amount of the flame retardant in the polymer, and reduces the production cost of the flame-retardant material. And the hydrotalcite is pre-intercalated, so that a high-molecular chain segment can enter between hydrotalcite layers to form a nano composite material, the compatibility with a polymer matrix is improved, and the mechanical property of the high-molecular composite material is improved. And the melamine polyphosphate is anchored on the surface of the hydrotalcite through an ion exchange reaction, so that the problem of mobility of the organic small-molecule flame retardant is solved, and the harm of secondary pollution in the using process is reduced. The inserted-layer hydrotalcite flame-retardant smoke suppressant disclosed by the invention does not contain halogen, has a good flame-retardant smoke suppressant effect and a wide application range, and meets the environmental protection requirement.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the present invention will be described in detail with reference to the accompanying drawings and detailed embodiments, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without inventive exercise. Wherein:
FIG. 1 is a reaction schematic diagram of the preparation of an intercalation type hydrotalcite flame-retardant smoke-suppressant of the invention;
FIG. 2 is an infrared spectrum of an intercalated hydrotalcite flame-retardant smoke suppressant of the present invention.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below.
Next, the present invention will be described in detail with reference to the drawings, wherein for convenience of illustration, the cross-sectional view of the device structure is not enlarged partially according to the general scale, and the drawings are only examples, which should not limit the scope of the present invention. In addition, the three-dimensional dimensions of length, width and depth should be included in the actual fabrication.
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be described in detail with reference to the accompanying drawings.
The invention provides an insertion-layer type hydrotalcite flame-retardant smoke suppressant, which does not contain halogen, has good flame-retardant and smoke-suppressant effects and wide application range and meets the requirement of environmental protection.
The inserted-layer hydrotalcite flame-retardant smoke suppressant comprises the following components in parts by mass: 1000g of distilled water, 100g of hydrotalcite, 6-20 g of dodecyl sulfopropyl betaine and 3-15 g of melamine polyphosphate. Preferably, in the embodiment, the composition comprises 1000g of distilled water, 100g of hydrotalcite, 20g of dodecyl sulfopropyl betaine and 15g of melamine polyphosphate according to the mass part ratio.
The preparation method of the intercalated hydrotalcite flame-retardant smoke suppressant is specifically described with reference to fig. 1-2.
Example 1
Adding 1L of distilled water and 100g of hydrotalcite into a stainless steel reaction kettle, carrying out ultrasonic dispersion for 30 minutes, adding 6g of dodecyl sulfopropyl betaine, stirring and reacting for 15 hours at 60 ℃, washing a product obtained by filtering for multiple times by using distilled water, and drying the obtained solid by blowing air to constant weight to obtain the dodecyl sulfopropyl betaine surface organic treatment hydrotalcite.
Adding 100g of the organic hydrotalcite surface treated by dodecyl sulfopropyl betaine into 1L of distilled water, ultrasonically dispersing for 30 minutes, transferring into a three-neck flask provided with a mechanical stirrer, a thermometer and a reflux condenser, dropwise adding a solution containing 3g of melamine polyphosphate/hydrochloric acid, wherein the pH value is 5.0, stirring and reacting for 8 hours at 25 ℃, filtering a suspension obtained by the reaction, washing with distilled water for three times, and drying in an oven at 100 ℃ for 24 hours to obtain the intercalated hydrotalcite flame-retardant smoke suppressant, wherein an infrared spectrogram is shown in figure 1.
Example 2
Adding 1L of distilled water and 100g of hydrotalcite into a stainless steel reaction kettle, carrying out ultrasonic dispersion for 30 minutes, adding 20g of dodecyl sulfopropyl betaine, stirring and reacting for 4 hours at 90 ℃, washing a product obtained by filtering for multiple times by using distilled water, and drying the obtained solid by blowing air to constant weight to obtain the dodecyl sulfopropyl betaine surface organic treatment hydrotalcite.
Adding 100g of the organic hydrotalcite surface treated by dodecyl sulfopropyl betaine into 1L of distilled water, ultrasonically dispersing for 30 minutes, transferring into a three-neck flask provided with a mechanical stirrer, a thermometer and a reflux condenser, dropwise adding a solution containing 15g of melamine polyphosphate/hydrochloric acid, wherein the pH value is 3.0, stirring and reacting for 2 hours at 60 ℃, filtering the suspension obtained by the reaction, washing with distilled water for three times, and drying in an oven at 100 ℃ for 24 hours to obtain the intercalated hydrotalcite flame-retardant smoke suppressant.
Example 3
Adding 1L of distilled water and 100g of hydrotalcite into a stainless steel reaction kettle, carrying out ultrasonic dispersion for 30 minutes, adding 15g of dodecyl sulfopropyl betaine, stirring and reacting for 6 hours at 70 ℃, washing a product obtained by filtering for multiple times by using distilled water, and drying the obtained solid by blowing air to constant weight to obtain the dodecyl sulfopropyl betaine surface organic treatment hydrotalcite.
Adding 100g of the organic hydrotalcite surface treated by dodecyl sulfopropyl betaine into 1L of distilled water, ultrasonically dispersing for 30 minutes, transferring into a three-neck flask provided with a mechanical stirrer, a thermometer and a reflux condenser, dropwise adding a solution containing 8g of melamine polyphosphate/hydrochloric acid, wherein the pH value is 4.5, stirring and reacting for 3 hours at 45 ℃, filtering the suspension obtained by the reaction, washing with distilled water for three times, and drying in an oven at 100 ℃ for 24 hours to obtain the intercalated hydrotalcite flame-retardant smoke suppressant.
Example 4
Adding 1L of distilled water and 100g of hydrotalcite into a stainless steel reaction kettle, carrying out ultrasonic dispersion for 30 minutes, adding 8g of dodecyl sulfopropyl betaine, stirring and reacting for 8 hours at 55 ℃, washing a product obtained by filtering for multiple times by using distilled water, and drying the obtained solid by blowing air to constant weight to obtain the dodecyl sulfopropyl betaine surface organic treatment hydrotalcite.
Adding 100g of the organic hydrotalcite surface treated by dodecyl sulfopropyl betaine into 1L of distilled water, ultrasonically dispersing for 30 minutes, transferring into a three-neck flask provided with a mechanical stirrer, a thermometer and a reflux condenser, dropwise adding a solution containing 6g of melamine polyphosphate/hydrochloric acid, wherein the pH value is 4.0, stirring and reacting for 5 hours at 30 ℃, filtering the suspension obtained by the reaction, washing with distilled water for three times, and drying in an oven at 100 ℃ for 24 hours to obtain the intercalated hydrotalcite flame-retardant smoke suppressant.
The prepared intercalated hydrotalcite flame-retardant smoke suppressant is used as a raw material to be processed into a material sample:
For comparison, the intercalated hydrotalcite flame-retardant smoke suppressant in the formula of the intercalated hydrotalcite/EPDM composite material is replaced by the same parts of the conventional intumescent flame retardant melamine polyphosphate, and the performance test results of the obtained flame-retardant EPDM are compared as follows:
as can be seen from the limit oxygen index value, the flame retardant level and the smoke density grade, compared with the conventional intumescent flame retardant melamine polyphosphate, the intercalated hydrotalcite flame retardant smoke suppressant can effectively improve the flame retardant and smoke suppressant performance of EPDM, and the mechanical property modification effect of EPDM is better than that of the intumescent flame retardant melamine polyphosphate. The intercalated hydrotalcite flame-retardant smoke suppressant used in the intercalated hydrotalcite/EPDM composite material prepared by the invention has good compatibility with the matrix material, has multiple functions of flame retardance, smoke suppression and reinforcement, and can improve the mechanical strength of the matrix material while modifying the flame retardance and the smoke suppression of the matrix material.
While the invention has been described above with reference to an embodiment, various modifications may be made and equivalents may be substituted for elements thereof without departing from the scope of the invention. In particular, the various features of the disclosed embodiments of the invention may be used in any combination, provided that no structural conflict exists, and the combinations are not exhaustively described in this specification merely for the sake of brevity and resource conservation. Therefore, it is intended that the invention not be limited to the particular embodiments disclosed, but that the invention will include all embodiments falling within the scope of the appended claims.
Claims (5)
1. The inserted hydrotalcite flame-retardant smoke suppressant is characterized by comprising the following components in parts by mass:
1000g of distilled water, 100g of hydrotalcite, 6-20 g of dodecyl sulfopropyl betaine and 3-15 g of melamine polyphosphate.
2. The intercalated hydrotalcite flame-retardant smoke suppressant according to claim 1, wherein the intercalated hydrotalcite comprises 1000g of distilled water, 100g of hydrotalcite, 20g of dodecyl sulfopropyl betaine and 15g of melamine polyphosphate in parts by mass.
3. The preparation method of the intercalated hydrotalcite flame-retardant smoke suppressant according to claim 1 or 2, which is characterized by comprising the following steps:
s1, uniformly dispersing hydrotalcite in a water phase, performing ultrasonic dispersion for 30 minutes, adding dodecyl sulfopropyl betaine, stirring and reacting for 4-15 hours at the temperature of 60-90 ℃, and separating to obtain the dodecyl sulfopropyl betaine surface organic treatment hydrotalcite;
s2, adding the organic surface treatment hydrotalcite of dodecyl sulfopropyl betaine into 1000g of distilled water, ultrasonically dispersing for 30 minutes, transferring into a three-neck flask provided with a mechanical stirrer, a thermometer and a reflux condenser tube, dropwise adding a melamine polyphosphate/hydrochloric acid solution with the pH value of 3.0-5.0, and stirring at 25-60 ℃ for reaction for 2-8 hours to obtain a suspension;
s3, filtering the suspension obtained by the reaction, washing the suspension for multiple times by using distilled water, and drying the suspension in an oven at 100 ℃ for 24 hours to obtain the intercalated hydrotalcite flame-retardant smoke suppressant.
4. The method for preparing an intercalated hydrotalcite flame-retardant smoke suppressant according to claim 1, wherein in step S1, the product obtained by filtration is washed with distilled water for a plurality of times, and the obtained solid is dried by forced air to constant weight to obtain the dodecylsulfopropyl betaine surface organically treated hydrotalcite.
5. The method of claim 1, wherein the suspension obtained from the reaction in step S3 is filtered and washed with distilled water three times.
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