CN114538484B - Preparation method of VOC modified filler mesoporous magnesium oxide for automotive interiors and PC composite material - Google Patents

Preparation method of VOC modified filler mesoporous magnesium oxide for automotive interiors and PC composite material Download PDF

Info

Publication number
CN114538484B
CN114538484B CN202210211882.0A CN202210211882A CN114538484B CN 114538484 B CN114538484 B CN 114538484B CN 202210211882 A CN202210211882 A CN 202210211882A CN 114538484 B CN114538484 B CN 114538484B
Authority
CN
China
Prior art keywords
magnesium oxide
voc
modified filler
composite material
mesoporous magnesium
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN202210211882.0A
Other languages
Chinese (zh)
Other versions
CN114538484A (en
Inventor
李卫红
袁超
张元君
孔俊
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Zhejiang Geely Holding Group Co Ltd
Geely Automobile Research Institute Ningbo Co Ltd
Original Assignee
Zhejiang Geely Holding Group Co Ltd
Geely Automobile Research Institute Ningbo Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Zhejiang Geely Holding Group Co Ltd, Geely Automobile Research Institute Ningbo Co Ltd filed Critical Zhejiang Geely Holding Group Co Ltd
Priority to CN202210211882.0A priority Critical patent/CN114538484B/en
Publication of CN114538484A publication Critical patent/CN114538484A/en
Application granted granted Critical
Publication of CN114538484B publication Critical patent/CN114538484B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F5/00Compounds of magnesium
    • C01F5/02Magnesia
    • C01F5/06Magnesia by thermal decomposition of magnesium compounds
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/02Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/04Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
    • B01J20/041Oxides or hydroxides
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • 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
    • 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
    • C08K7/26Silicon- containing compounds
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2253/00Adsorbents used in seperation treatment of gases and vapours
    • B01D2253/10Inorganic adsorbents
    • B01D2253/106Silica or silicates
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2253/00Adsorbents used in seperation treatment of gases and vapours
    • B01D2253/10Inorganic adsorbents
    • B01D2253/112Metals or metal compounds not provided for in B01D2253/104 or B01D2253/106
    • B01D2253/1124Metal oxides
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2257/00Components to be removed
    • B01D2257/70Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
    • B01D2257/708Volatile organic compounds V.O.C.'s
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00Aspects relating to sorbent materials
    • B01J2220/40Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48Sorbents characterised by the starting material used for their preparation
    • B01J2220/4806Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/64Nanometer sized, i.e. from 1-100 nanometer
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/12Surface area
    • 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
    • C08K2201/00Specific properties of additives
    • C08K2201/011Nanostructured additives
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02ATECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/20Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Nanotechnology (AREA)
  • Manufacturing & Machinery (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • General Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Thermal Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

The invention relates to a preparation method of VOC modified filler mesoporous magnesium oxide for automotive interiors and a PC composite material, belonging to the technical field of automotive interiors. In order to solve the problems of poor adsorptivity and difficult preparation, the preparation method of the VOC modified filler mesoporous magnesium oxide for the automotive interior is provided, and the method comprises the steps of adding magnesium ammonium sulfate and ammonium bicarbonate into water, and controlling the temperature to be 30-50 ℃ for reaction to form a solution containing solid intermediate state; filtering the solution containing the solid intermediate state to obtain an intermediate state solid, and calcining at the temperature of 700-800 ℃ to obtain the VOC modified filler mesoporous magnesium oxide; the PC composite material comprises the following components in parts by weight: PC: 80-100; VOC modified filler mesoporous magnesium oxide: 8-12; an antioxidant: 0.1 to 0.5. The material obtained by the invention has the characteristics of small particle size and large specific surface area, and can effectively adsorb VOC (volatile organic compounds) and has high stability.

Description

Preparation method of VOC modified filler mesoporous magnesium oxide for automotive interiors and PC composite material
Technical Field
The invention relates to a preparation method of VOC modified filler mesoporous magnesium oxide for automotive interiors and a PC composite material, belonging to the technical field of automotive interiors.
Background
The national control of automobile VOCs is becoming more stringent, and the demand for low odor plastic materials is increasing within the industry. The odor level requirements have been included in one of the primary indicators in many automotive fitting enterprises. At present, automobile interiors are mainly made of materials such as Polycarbonate (PC), PVC and the like, strong pungent smell can be emitted in the use process, and when volatilized gas reaches a certain concentration in an automobile, people in the automobile feel uncomfortable and bad influence on the health is generated.
In the specific application fields of automobiles and the like, the VOC performance requirements of the materials are higher and higher, the requirements of common PC materials and the like cannot be met, and the application of the PC materials and the like in the specific fields is limited to a certain extent. Therefore, in order to solve the odor problem of emitting VOC around the plastic material for automotive interior, the odor absorbing material such as zeolite and molecular sieve is mainly added into the plastic material to adsorb volatile gases of small molecules in a physical or chemical manner, but how to achieve the low VOC odor effect is not ideal in practical application. This requires that the adsorption be made of what material is used as an additive to ensure the performance of achieving low VOC odors.
The magnesium oxide particles as the adsorption material have better physical and chemical properties, which are incomparable with other materials, but the magnesium oxide prepared by the conventional method still has the problem of unsatisfactory adsorption performance, such as weak adsorption capacity, and is unfavorable for effectively adsorbing VOC gas. Magnesium hydroxide is usually prepared in the preparation of magnesium oxide materials as in the prior art, and then mesoporous magnesium oxide is formed by calcination. The mesoporous magnesia prepared by the method has poor pore-forming property and weak adsorption capability to VOC, and also has a soft template method which takes amphiphilic organic molecules or block copolymers as templates, but because magnesium ions have low hydrolysis speed under alkaline conditions and effective acting force is difficult to form between the magnesium ions and the templates, the mesoporous magnesia is not easy to prepare.
Disclosure of Invention
Aiming at the problems existing in the prior art, the invention provides a preparation method of VOC modified filler mesoporous magnesium oxide for automotive interiors and a PC composite material, and solves the problems of realizing the performances of high VOC adsorption capacity and easiness in synthesis.
The invention discloses a preparation method of VOC modified filler mesoporous magnesium oxide for automotive interiors, which comprises the following steps:
A. adding magnesium ammonium sulfate and ammonium bicarbonate into water for mixing, and controlling the temperature to be 30-50 ℃ for reaction treatment to form corresponding solution containing solid intermediate state;
B. filtering the obtained solution containing the solid intermediate state to obtain a corresponding intermediate state solid, and calcining at the temperature of 700-800 ℃ to obtain the corresponding VOC modified filler mesoporous magnesium oxide.
By taking magnesium ammonium sulfate and ammonium bicarbonate as raw materials and carrying out reaction treatment at the temperature of 30-50 ℃, the method can form a middle state completely different from the conventional middle state, so that corresponding middle state solid matters are formed, the method is beneficial to effectively decomposing and forming mesoporous magnesia in the subsequent calcination process, gas generated in the decomposition process of middle state matters in the calcination process can effectively form a pore microstructure, part of the formed gas can be decomposed and diffused outwards from the inside, the porosity of the formed mesoporous magnesia is effectively improved, the excellent effects of small super-large specific surface area and particle size and good dispersibility are realized, the adsorption capacity to VOC smell is realized, and the method also has the advantage of strong adsorption capacity. The reaction temperature is preferably controlled at 40-45 ℃, which is more favorable for the reaction and effectively forms corresponding intermediate products, has the effect of high purity and quality, and the improvement of purity is more favorable for forming excellent porosity and specific surface area in the subsequent calcination process and improves the overall adsorption performance. The additive applied to the PC material can also realize the performance of low VOC, realize the effect of effectively controlling VOC, and the raw materials adopted by the method are synthesized into a middle state and calcined, so that the preparation without adopting a template sheet can be realized, and the preparation method is more beneficial to realizing the advantages of simple operation and easiness in synthesis.
In the above method for preparing the VOC-modified filler mesoporous magnesium oxide for automotive interior, preferably, the solid intermediate state in step a is NH 4 MgOHCO 3 A solid. The intermediate state substance can be formed by selecting raw materials and effectively controlling the reaction temperature, and the aim is to ensure that the formed intermediate state substance contains amino groups, carbonate groups and other groups, so that sufficient gas substances can be formed by decomposition in the calcining process, and the formed magnesium oxide can better generate pores by volatilizing the gas substances, thereby more effectively ensuring that the generated mesoporous magnesium oxide has excellent porosity, has the effect of high specific surface area, has good dispersibility in preparation and has the advantage of small particle size. The reaction principle in the above-mentioned mesoporous magnesium oxide production process can be explained by the following manner (hereinafter, using (NH) 4 ) 2 Mg(SO 4 ) 2 To represent magnesium ammonium sulphate):
(NH 4 ) 2 Mg(SO 4 ) 2 +3NH 4 HCO 3 →NH 4 MgOHCO 3 +2(NH 4 ) 2 SO 4 +2CO 2 +H 2 O
NH 4 MgOHCO 3 →MgO+NH 3 +H 2 O+CO 2
namely, the intermediate solid product in the step A is formed by the reaction principle to form corresponding intermediate characteristics, so that the mesoporous magnesium oxide which is favorable for the subsequent calcination process has excellent performance.
In the above preparation method of the VOC-modified filler mesoporous magnesium oxide for automotive interior, preferably, the ammonium magnesium sulfate in step a: the mass ratio of the ammonium bicarbonate is 30-40: 24-30. The reaction is more fully carried out, which is beneficial to improving the overall utilization rate of the raw materials. Further preferably, the magnesium ammonium sulfate: ammonium bicarbonate: the mass ratio of the water is 30-40: 24-30: 60 to 80 percent. Deionized water is preferably used for the water.
In the above method for producing a VOC-modified filler mesoporous magnesium oxide for automotive interiors, the reaction treatment in step a is preferably for 4 to 6 hours. The reaction can be fully carried out, and the conversion rate of raw materials and the yield of intermediate products are improved.
In the above method for producing a VOC-modified filler mesoporous magnesium oxide for automotive interiors, the calcination treatment in step B is preferably performed for 10 to 16 hours.
The second object of the invention is realized by the following technical scheme, and the PC composite material for the automotive interior is characterized by comprising the following components in parts by weight:
PC: 80-100; VOC modified filler mesoporous magnesium oxide: 8-12; an antioxidant: 0.1 to 0.5; the VOC modified filler mesoporous magnesium oxide is prepared by the following method:
adding magnesium ammonium sulfate and ammonium bicarbonate into water for mixing, and controlling the temperature to be 30-50 ℃ for reaction treatment to form corresponding solution containing solid intermediate state;
filtering the obtained solution containing the solid intermediate state to obtain a corresponding intermediate state solid, and calcining at the temperature of 700-800 ℃ to obtain the corresponding VOC modified filler mesoporous magnesium oxide.
The mesoporous magnesium oxide prepared by the method is added into the PC plastic (polycarbonate) material, has the excellent properties of large specific surface area and high porosity, can effectively play a role in adsorption, and reduces the property of low VOC when being used as an automobile interior material, thereby effectively improving the use of the mesoporous magnesium oxide. Other additive assistants such as light stabilizer and the like can be further added into the PC composite material, so that the corresponding performance of the material is improved.
In the PC composite material for automobile interior trim, the antioxidant is preferably one or more selected from phenyl tris (2, 4-di-t-butyl) phosphite (abbreviated as Irganox 168), pentaerythritol tetrakis [ β - (3, 5-di-t-butyl-4-hydroxyphenyl) propionate (abbreviated as Irganox 1010), and 1,3, 5-trimethyl-2, 4,6- (3, 5-di-t-butyl-4-hydroxybenzyl) benzene (abbreviated as Irganox 1330). The aging resistance of the PC composite material can be effectively improved, and the service life of the PC composite material is prolonged. As a further preferred, the antioxidant is a mixture of phenyl tris (2, 4-di-t-butyl) phosphite, pentaerythritol tetrakis [ β - (3, 5-di-t-butyl-4-hydroxyphenyl) propionate ] and 1,3, 5-trimethyl-2, 4,6- (3, 5-di-t-butyl-4-hydroxybenzyl) benzene, and the mass ratio of phenyl tris (2, 4-di-t-butyl) phosphite, pentaerythritol tetrakis [ β - (3, 5-di-t-butyl-4-hydroxyphenyl) propionate ] and 1,3, 5-trimethyl-2, 4,6- (3, 5-di-t-butyl-4-hydroxybenzyl) benzene is 1:1.8 to 2.0:1.5 to 2.1.
In the PC composite material for automobile interior trim, it is preferable that the PC composite material further includes 1.0 to 1.2 parts by weight of nano-sized porous calcium silicate. Because of high VOC requirements as automotive interiors, the adsorption performance of the nano porous calcium silicate on formaldehyde, acetaldehyde and other aldehyde volatile gases can be improved by adding a small amount of nano porous calcium silicate. As a further preferred aspect, the nano-scale porous calcium silicate has a particle size of 10nm to 15nm. Further, it is preferable to have the porosity of the nano-porous calcium silicate be 82% to 88%.
In the PC composite material for the automotive interior, the PC composite material can be prepared by the following method:
according to the proportion of the raw materials, 80 to 100 parts by weight of PC, 8 to 12 parts by weight of VOC modified filler mesoporous magnesium oxide and 0.1 to 0.5 part by weight of antioxidant are weighed, mixed and stirred uniformly to obtain a mixture;
and adding the obtained mixture into a double-screw extruder for extrusion granulation to obtain the corresponding PC composite material.
In the PC composite material for automotive interior, preferably, the twin-screw extruder includes six temperature zones arranged in sequence at the time of extrusion granulation, and the temperature setting control is: the temperature of the first area is 200-220 ℃, the temperature of the second area is 250-270 ℃, the temperature of the third area is 250-270 ℃, the temperature of the fourth area is 250-270 ℃, the temperature of the fifth area is 250-270 ℃, the temperature of the sixth area is 250-270 ℃, the temperature of the machine head is 250-270 ℃, and the rotating speed of the screw is 200-280 r/min. Better guarantee extrusion effect.
In summary, compared with the prior art, the invention has the following advantages:
1. the intermediate state formed by the reaction of the magnesium ammonium sulfate and the ammonium bicarbonate is utilized as raw materials, so that the calcination process is more favorable for forming mesoporous magnesium oxide with excellent performance, the preparation and the operation are easy, the obtained mesoporous magnesium oxide has the characteristics of small particle size and large specific surface area, the VOC adsorption performance can be effectively realized, and the adsorption stability is high.
2. By adding a small amount of nano porous calcium silicate, the adsorption performance of the nano porous calcium silicate on formaldehyde, acetaldehyde and other aldehyde volatile gases can be better improved, and the performance of the PC composite material is improved.
Detailed Description
The technical scheme of the present invention will be further specifically described by means of specific examples, but the present invention is not limited to these examples.
Example 1
According to the proportion of the dosage of each raw material, 300g of magnesium ammonium sulfate, 240g of ammonium bicarbonate and 600g of deionized water are weighed and put into a reaction vessel, then the temperature of the system is controlled at 30 ℃ for reaction treatment for 4 hours, and after the reaction is finished, an intermediate product NH is obtained 4 MgOHCO 3 Is a solution of (a);
then the intermediate product NH is contained 4 MgOHCO 3 Filtering, washing and drying the solution of the catalyst to obtain a corresponding intermediate product, and then placing the intermediate product in a muffle furnace at 700 ℃ for calcination treatment for 10 hours to obtain the corresponding product VOC modified filler mesoporous magnesium oxide. The particle diameter of the particles reaches 10nm, and the specific surface area reaches 331m 2 /g。
Example 2
The PC composite material for the automotive interior comprises the following components in parts by weight:
PC (polycarbonate): 80; VOC modified filler mesoporous magnesium oxide: 8, 8; irganox1010:0.1.
weighing the raw materials according to the weight proportion of the raw materials, weighing 80 parts by weight of PC, 8 parts by weight of VOC modified filler mesoporous magnesium oxide and 0.1 part by weight of Irganox1010, mixing and stirring uniformly to obtain corresponding mixture, wherein the VOC modified filler mesoporous magnesium oxide is obtained by adopting the method of the embodiment 1;
extruding and granulating the obtained mixture in a double-screw extruder to obtain a PC composite material (named as PC composite material P1) for automobile interior trim; the twin-screw extruder comprises six temperature areas which are sequentially arranged, wherein the temperature of the first area is 200 ℃, the temperature of the second area is 250 ℃, the temperature of the third area is 250 ℃, the temperature of the fourth area is 250 ℃, the temperature of the fifth area is 250 ℃, the temperature of the sixth area is 250 ℃, the temperature of the machine head is 250-270 ℃, and the rotating speed of the screw is 200r/min.
Example 3
According to the proportion of the raw materials, 350g of magnesium ammonium sulfate, 270g of ammonium bicarbonate and 700g of deionized water are weighed and put into a reaction vessel, then the temperature of the system is controlled at 40 ℃ for reaction treatment for 5 hours, and after the reaction is finished, an intermediate product NH is obtained 4 MgOHCO 3 Is a solution of (a);
then the intermediate product NH is contained 4 MgOHCO 3 Filtering, washing and drying the solution of the catalyst to obtain a corresponding intermediate product, and then placing the intermediate product in a muffle furnace at 740 ℃ for calcination treatment for 16 hours to obtain the corresponding product VOC modified filler mesoporous magnesium oxide. The particle diameter of the particles reaches 12nm, and the specific surface area reaches 335m 2 /g。
Example 4
The PC composite material for the automotive interior comprises the following components in parts by weight:
PC (polycarbonate): 90; VOC modified filler mesoporous magnesium oxide: 10; irganox1010:0.1; irganox168:0.1; the VOC-modified filler mesoporous magnesium oxide herein was obtained by the method of example 3 described above.
The PC composite material for automotive interior according to this embodiment is prepared by the corresponding method in embodiment 2, and will not be described here again, and the obtained PC composite material for automotive interior (designated as PC composite material P2).
Example 5
According to the proportion of the dosage of each raw material, 400g of magnesium ammonium sulfate, 300g of ammonium bicarbonate and 800g of deionized water are weighed and put into a reaction vessel, then the temperature of the system is controlled at 50 ℃ for reaction treatment for 6 hours, and after the reaction is finished, an intermediate product NH is obtained 4 MgOHCO 3 Is a solution of (a);
then the intermediate product NH is contained 4 MgOHCO 3 Filtering, washing and drying the solution of the catalyst to obtain a corresponding intermediate product, and then placing the intermediate product in a muffle furnace at 800 ℃ for calcining for 15 hours to obtain the corresponding product VOC modified filler mesoporous magnesium oxide. The particle diameter of the particles reaches 13nm, and the specific surface area reaches 330m 2 /g。
Example 6
The PC composite material for the automotive interior comprises the following components in parts by weight:
PC (polycarbonate): 100; VOC modified filler mesoporous magnesium oxide: 12; irganox1010:0.2; irganox168:0.1; irganox1330:0.2; the VOC-modified filler mesoporous magnesium oxide herein was obtained by the method of example 5 described above.
The PC composite material for automotive interior according to this embodiment is prepared by the corresponding method in embodiment 2, and will not be described here again, and the obtained PC composite material for automotive interior (designated as PC composite material P3).
Example 7
According to the proportion of the dosage of each raw material, 325g of magnesium ammonium sulfate, 275g of ammonium bicarbonate and 635g of deionized water are weighed and put into a reaction vessel, then the temperature of the system is controlled at 35 ℃ for reaction treatment for 5 hours, and after the reaction is finished, an intermediate product NH is obtained 4 MgOHCO 3 Is a solution of (a);
then the intermediate product NH is contained 4 MgOHCO 3 Filtering, washing and drying the solution of the catalyst to obtain a corresponding intermediate product, and then placing the intermediate product into a 745 ℃ muffle furnace for calcination treatment for 14 hours to obtain the corresponding product VOC modified filler mesoporous magnesium oxide. The particle diameter of the particles reaches 11nm, and the specific surface area reaches 335m 2 /g。
Example 8
The PC composite material for the automotive interior comprises the following components in parts by weight:
PC (polycarbonate): 85; VOC modified filler mesoporous magnesium oxide: 11; irganox1010:0.1; the VOC-modified filler mesoporous magnesium oxide herein was obtained by the method of example 7 above.
The PC composite material for automotive interior according to this embodiment is prepared by the corresponding method in embodiment 2, and will not be described here again, and the obtained PC composite material for automotive interior (designated as PC composite material P4) is obtained.
Example 9
According to the proportion of the raw materials, 385g of magnesium ammonium sulfate, 275g of ammonium bicarbonate and 755g of deionized water are weighed and put into a reaction vessel, then the temperature of the system is controlled at 40 ℃ for reaction treatment for 4 hours, and after the reaction is finished, an intermediate product NH is obtained 4 MgOHCO 3 Is a solution of (a);
then the intermediate product NH is contained 4 MgOHCO 3 Filtering, washing and drying the solution of the catalyst to obtain a corresponding intermediate product, and then placing the intermediate product into a 745 ℃ muffle furnace for calcining for 15 hours to obtain the corresponding product VOC modified filler mesoporous magnesium oxide. The particle diameter of the particles reaches 12nm, and the specific surface area reaches 333m 2 /g。
Example 10
The PC composite material for the automotive interior comprises the following components in parts by weight:
PC (polycarbonate): 85; VOC modified filler mesoporous magnesium oxide: 12; irganox1010:0.3; the VOC-modified filler mesoporous magnesium oxide was obtained by the method of example 9 described above, and the obtained PC composite material for automobile interior trim (designated as PC composite material P5) was obtained.
Example 11
The PC composite material for the automotive interior comprises the following components in parts by weight:
PC (polycarbonate): 100; VOC modified filler mesoporous magnesium oxide: 12; irganox1010:0.2; irganox168:0.1; irganox1330:0.2; nanoscale porous calcium silicate: 1.2; the nano-scale porous calcium silicate had a particle size of 10nm and a porosity of 85%, and the VOC-modified filler mesoporous magnesium oxide was obtained by the method of example 5 described above, to obtain a PC composite material for automobile interior trim (designated as PC composite material P6).
Example 12
The PC composite material for the automotive interior comprises the following components in parts by weight:
PC (polycarbonate): 90; VOC modified filler mesoporous magnesium oxide: 10; irganox1010:0.1; nanoscale porous calcium silicate: 1.0; the nano-scale porous calcium silicate had a particle size of 12nm and a porosity of 82%, and the VOC-modified filler mesoporous magnesium oxide was obtained by the method of example 3 described above, to obtain a PC composite material for automobile interior trim (designated as PC composite material P7).
Example 13
The PC composite material for the automotive interior comprises the following components in parts by weight:
PC (polycarbonate): 85; VOC modified filler mesoporous magnesium oxide: 11; irganox1010:0.1; nanoscale porous calcium silicate: 1.3; the nano-scale porous calcium silicate had a particle size of 15nm and a porosity of 88%, and the VOC-modified filler mesoporous magnesium oxide was obtained by the method of example 7 described above, to obtain a PC composite material for automobile interior trim (designated as PC composite material P8).
Comparative example 1
The PC composite material for the automotive interior comprises the following components in parts by weight:
PC (polycarbonate): 85; irganox1010:0.1.
according to the proportion of the raw materials, 85 parts by weight of PC and 0.1 part by weight of Irganox1010 are weighed and mixed uniformly to obtain a mixture;
and (3) putting the obtained mixture into a double-screw extruder for extrusion granulation to obtain the PC composite material (named as PC composite material D1). The twin-screw extruder comprises six temperature areas which are sequentially arranged, wherein the temperature of the first area is 215 ℃, the temperature of the second area is 265 ℃, the temperature of the third area is 265 ℃, the temperature of the fourth area is 265 ℃, the temperature of the fifth area is 265 ℃, the temperature of the sixth area is 265 ℃, the temperature of the machine head is 265 ℃, and the rotating speed of the screw is 245r/min.
The performance test was carried out by randomly selecting the corresponding PC composite materials obtained in the above examples 2,4,6, 8 and 10-13 and the VOC of the PC composite materials obtained in the corresponding comparative example 1, and the test standard was GB/T27630, and the specific test results are shown in tables 1 and 2:
table 1:
the PC composites P1 and P2 obtained in the corresponding example 2 and the PC composites P2 and P3 obtained in the corresponding example 4 and the PC composites P3 and P4 obtained in the corresponding example 6 and the PC composites P4 and P5 obtained in the corresponding example 8 and the PC composite P5 obtained in the corresponding example 10 in table 1.
Table 2:
in table 2, P6 corresponds to the PC composite material P6 and P7 obtained in example 11, P7 corresponds to the PC composite material P7 obtained in example 12, P8 corresponds to the PC composite material P8 obtained in example 13, and D1 corresponds to the PC composite material D1 obtained in comparative example 1, wherein ND indicates undetected.
The test results in the above tables 1 and 2 show that the PC composite material adopting the invention has excellent low VOC performance, and the addition of a small amount of nano-scale porous calcium silicate can lead to better adsorption performance on aldehyde volatile odor and better low VOC performance effect.
The specific embodiments described herein are offered by way of illustration only. Those skilled in the art may make various modifications or additions to the described embodiments or substitutions thereof without departing from the spirit of the invention or exceeding the scope of the invention as defined in the accompanying claims.
While the invention has been described in detail and with reference to specific embodiments thereof, it will be apparent to one skilled in the art that various changes and modifications can be made therein without departing from the spirit and scope thereof.

Claims (9)

1. The preparation method of the VOC modified filler mesoporous magnesium oxide for the automotive interiors is characterized by comprising the following steps of:
A. adding magnesium ammonium sulfate and ammonium bicarbonate into water for mixing, and controlling the temperature to be 30-50 ℃ for reaction treatment to form corresponding solution containing solid intermediate state; the magnesium ammonium sulfate: the mass ratio of the ammonium bicarbonate is 30-40: 24-30;
B. filtering the obtained solution containing the solid intermediate state to obtain a corresponding intermediate state solid, and calcining at the temperature of 700-800 ℃ to obtain the corresponding VOC modified filler mesoporous magnesium oxide.
2. The method for preparing the VOC-modified mesoporous magnesium oxide for automotive interiors according to claim 1, wherein in the step A, the solid intermediate state is NH 4 MgOHCO 3 A solid.
3. The method for preparing the VOC-modified filler mesoporous magnesium oxide for automotive interiors according to claim 1 or 2, wherein the reaction treatment time in step a is 4 to 6 hours.
4. The method for producing a VOC-modified filler mesoporous magnesium oxide for automotive interiors according to claim 1 or 2, characterized in that the calcination treatment in step B is performed for 10 to 16 hours.
5. The PC composite material for the automotive interior is characterized by comprising the following components in parts by weight:
PC: 80-100; VOC modified filler mesoporous magnesium oxide: 8-12; an antioxidant: 0.1 to 0.5; the VOC modified filler mesoporous magnesium oxide is prepared by the following method:
adding magnesium ammonium sulfate and ammonium bicarbonate into water for mixing, and controlling the temperature to be 30-50 ℃ for reaction treatment to form corresponding solution containing solid intermediate state; the magnesium ammonium sulfate: the mass ratio of the ammonium bicarbonate is 30-40: 24-30;
filtering the obtained solution containing the solid intermediate state to obtain a corresponding intermediate state solid, and calcining at the temperature of 700-800 ℃ to obtain the corresponding VOC modified filler mesoporous magnesium oxide.
6. The PC composite material for automotive interiors according to claim 5, wherein the antioxidant is one or more selected from the group consisting of phenyl tris (2, 4-di-t-butyl) phosphite, pentaerythritol tetrakis [ β - (3, 5-di-t-butyl-4-hydroxyphenyl) propionate ] and 1,3, 5-trimethyl-2, 4,6- (3, 5-di-t-butyl-4-hydroxybenzyl) benzene.
7. The PC composite material for automotive interiors according to claim 5 or 6, wherein the antioxidant is a mixture of phenyl tris (2, 4-di-t-butyl) phosphite, pentaerythritol tetrakis [ β - (3, 5-di-t-butyl-4-hydroxyphenyl) propionate ] and 1,3, 5-trimethyl-2, 4,6- (3, 5-di-t-butyl-4-hydroxybenzyl) benzene, and the mass ratio of phenyl tris (2, 4-di-t-butyl) phosphite, pentaerythritol tetrakis [ β - (3, 5-di-t-butyl-4-hydroxyphenyl) propionate ] and 1,3, 5-trimethyl-2, 4,6- (3, 5-di-t-butyl-4-hydroxybenzyl) benzene is 1:1.8 to 2.0:1.5 to 2.1.
8. The PC composite for automotive interiors according to claim 5 or 6, further comprising 1.0 to 1.2 parts by weight of nano-sized porous calcium silicate.
9. The PC composite for automotive interiors according to claim 8, wherein the nano-sized porous calcium silicate has a particle size of 10nm to 15nm.
CN202210211882.0A 2022-03-04 2022-03-04 Preparation method of VOC modified filler mesoporous magnesium oxide for automotive interiors and PC composite material Active CN114538484B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202210211882.0A CN114538484B (en) 2022-03-04 2022-03-04 Preparation method of VOC modified filler mesoporous magnesium oxide for automotive interiors and PC composite material

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202210211882.0A CN114538484B (en) 2022-03-04 2022-03-04 Preparation method of VOC modified filler mesoporous magnesium oxide for automotive interiors and PC composite material

Publications (2)

Publication Number Publication Date
CN114538484A CN114538484A (en) 2022-05-27
CN114538484B true CN114538484B (en) 2023-11-24

Family

ID=81661097

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202210211882.0A Active CN114538484B (en) 2022-03-04 2022-03-04 Preparation method of VOC modified filler mesoporous magnesium oxide for automotive interiors and PC composite material

Country Status (1)

Country Link
CN (1) CN114538484B (en)

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB763451A (en) * 1952-10-06 1956-12-12 Wintershall Ag Process for the preparation of easily-filtrable magnesia and ammonium sulphate
CN102424431A (en) * 2011-09-01 2012-04-25 东北大学 Method for preparing nickel oxide, magnesium oxide and silicon oxide products from laterite-nickel ore
CN106564919A (en) * 2016-11-08 2017-04-19 贵州省化工研究院 Method for directly preparing magnesium ammonium sulfate through phosphorite magnesium removal
CN112919509A (en) * 2021-04-09 2021-06-08 东北大学 Method for producing ammonium magnesium sulfate and basic magnesium carbonate based on boron sludge
CN113072094A (en) * 2021-03-22 2021-07-06 安徽江淮汽车集团股份有限公司 Polyolefin VOC (volatile organic compound) improved filler, preparation method thereof and polyolefin composite material

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB763451A (en) * 1952-10-06 1956-12-12 Wintershall Ag Process for the preparation of easily-filtrable magnesia and ammonium sulphate
CN102424431A (en) * 2011-09-01 2012-04-25 东北大学 Method for preparing nickel oxide, magnesium oxide and silicon oxide products from laterite-nickel ore
CN106564919A (en) * 2016-11-08 2017-04-19 贵州省化工研究院 Method for directly preparing magnesium ammonium sulfate through phosphorite magnesium removal
CN113072094A (en) * 2021-03-22 2021-07-06 安徽江淮汽车集团股份有限公司 Polyolefin VOC (volatile organic compound) improved filler, preparation method thereof and polyolefin composite material
CN112919509A (en) * 2021-04-09 2021-06-08 东北大学 Method for producing ammonium magnesium sulfate and basic magnesium carbonate based on boron sludge

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
李洁 ; 申晓毅 ; 张杰 ; 翟玉春 ; .由硫酸镁铵溶液制备Mg(OH)_2的实验研究.轻金属.2018,(第08期),全文. *
由硫酸镁铵溶液制备Mg(OH)_2的实验研究;李洁;申晓毅;张杰;翟玉春;;轻金属(第08期);全文 *

Also Published As

Publication number Publication date
CN114538484A (en) 2022-05-27

Similar Documents

Publication Publication Date Title
CN103724799B (en) A kind of low smell, low diffusion polypropylene composition and preparation method thereof
CN103739944B (en) A kind of low smell glass fiber reinforced polypropylene composite material and preparation method thereof
CN105037941B (en) A kind of low VOC, low smell wood-fibred reinforced polypropylene compound material and preparation method thereof
CN105602096B (en) It is a kind of for the low volatility PP composite material of automotive interior material and its preparation and method
CN104710688A (en) Low-odor high-performance polypropylene composite material and preparation method thereof
CN104693471B (en) Multi-functional perforate expanded polymer particles and preparation method thereof
CN103772884A (en) Low-odor and low-emission acrylonitrile-butadiene-styrene (ABS) composition and preparation method thereof
CN103724921B (en) A kind of low smell, lowly distribute, antibacterial ABS composition and method of making the same
JP7479477B2 (en) Low odor soft PVC material
CN103724923A (en) Antibacterial ABS (Acrylonitrile Butadiene Styrene) composite material with low smell and low diffusion and preparation method thereof
CN109721844A (en) A kind of high antibacterial low distributes automobile-used modified polypropylene composite material and preparation method thereof
CN102382363A (en) Modified polypropylene material and preparation method thereof
CN103709704B (en) A kind of low smell, lowly distribute PC/ABS Alloy And Preparation Method
CN113248829A (en) Low-odor polypropylene composition and preparation method and application thereof
CN106928552A (en) It is a kind of with antibacterial, remove automotive upholstery modified polypropylene material for eliminating the unusual smell and preparation method thereof
CN109957172A (en) A kind of eliminating smell agent, it is low distribute, automobile interior decoration polypropylene material resistant to high temperature and preparation method thereof
CN112574440A (en) Adsorption type low-odor master batch for polypropylene and preparation method thereof
CN105566750B (en) Except volatile substance master batch, the low volatilization automobile interior decoration composite material of low smell and preparation method
CN112143185A (en) Antibacterial and deodorant polyester master batch, manufacturing method thereof and polyester fiber
CN114538484B (en) Preparation method of VOC modified filler mesoporous magnesium oxide for automotive interiors and PC composite material
CN103740020B (en) A kind of low abnormal smells from the patient fiberglass reinforced AS composition and method of making the same
CN109694521A (en) A kind of low VOC Low-odor polypropylene resin composition and preparation method thereof
CN109694524A (en) A kind of polypropylene resin composite and preparation method thereof of the low smell of low VOC
KR20180038810A (en) Material for reducing volatile organic compounds and manufacturing method thereof
CN115873346A (en) Low-odor polypropylene master batch and preparation method and application thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant