CN104829961A - Preparation method of rare earth thermal-stabilizer - Google Patents
Preparation method of rare earth thermal-stabilizer Download PDFInfo
- Publication number
- CN104829961A CN104829961A CN201410744121.7A CN201410744121A CN104829961A CN 104829961 A CN104829961 A CN 104829961A CN 201410744121 A CN201410744121 A CN 201410744121A CN 104829961 A CN104829961 A CN 104829961A
- Authority
- CN
- China
- Prior art keywords
- rare earth
- preparation
- sodium hydroxide
- stabilizer
- distilled water
- 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.)
- Pending
Links
Classifications
-
- 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
- C08K5/04—Oxygen-containing compounds
- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
- C08K5/098—Metal salts of carboxylic acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
A preparation method of a rare earth thermal-stabilizer belongs to the field of preparation of materials and includes the steps of: (a) weighing a carboxylic acid rare earth salt, a nitric acid rare earth salt and sodium hydroxide; (b) dissolving the carbolic acid rare earth salt and the nitric acid rare earth salt respectively in proper amounts of anhydrous alcohol and distilled water, adding the solution into a flask by one time, assembling a reflux water bath heating device and stirring the solution; (c) adding the sodium hydroxide to a constant-pressure dropping funnel and dropwisely adding the sodium hydroxide slowly to the mixed solution, and performing a reaction for half an hour after the sodium hydroxide added dropwisely; and (d) performing vacuum filtration after the reaction finished, washing a reaction product with anhydrous alcohol and distilled water, and drying the reaction product to obtain a white or almost white powder which is the product. By means of effective improvement of raw materials and preparation processes, the rare earth thermal-stabilizer is excellent in thermal stability and has a wide synergistic effect when being matched with other thermal-stabilizer so that thermal stability and processability of PVC can be effectively enhanced. The preparation method is simple in operation, is low in raw material cost, can save cost, and has a great market popularization value.
Description
Technical field
The invention belongs to field of material preparation, particularly relate to a kind of preparation method of rare earth thermal stabilizer.
Background technology
Along with the development of science and technology, increasing novel material occurs and is applied in life, the appearance of the various new technique of simultaneous, thermo-stabilizer is that one can prevent or reduce polyvinyl chloride (PVC) resin crosslinked or degraded occurs because being heated in the course of processing, extends the important additives in its goods work-ing life.The thermo-stabilizer that the current usage quantity of China market is larger has lead salts, metal soap and organic tin.Lead salts cost is low and effective, but is prohibitted the use gradually in some PVC goods because of its toxicity; Metal soap easy generation as Zinic stearas is used alone " zinc burning " phenomenon; The problem that organic tin is then on the high side, have impact on the development of relevant industries to a certain extent.
Summary of the invention
The present invention is intended to solve the problem, and provides a kind of preparation method of rare earth thermal stabilizer.
A preparation method for rare earth thermal stabilizer, is characterized in that comprising the steps:
(1) carboxylic acid, rare earth nitrate salt and sodium hydroxide is taken by amount of substance than 1:1:3;
(2) carboxylic acid, rare earth nitrate salt are dissolved with appropriate dehydrated alcohol and distilled water respectively, disposablely add in three-necked flask, assembling backflow water bath heating device, starts electric stirring;
(3) then sodium hydroxide solution is loaded constant pressure funnel, be slowly added drop-wise in mixing solutions, dropwise rear continuation and react half an hour;
(4) reaction terminates after product vacuum filtration, with dehydrated alcohol and the distilled water wash of heat, dry, obtains white or near-white powder and is product.
The preparation method of a kind of rare earth thermal stabilizer of the present invention, is characterized in that described in step (2), bath temperature is 80 DEG C.
The preparation method of a kind of rare earth thermal stabilizer of the present invention, is characterized in that described in step (1), rare earth nitrate salt comprises lanthanum nitrate, cerous nitrate and neodymium nitrate.
The preparation method of a kind of rare earth thermal stabilizer of the present invention, is characterized in that the washing times of distilled water described in step (4) is 4 times.
The preparation method of a kind of rare earth thermal stabilizer of the present invention, by the effective improvement to raw materials and technique, make the thermo-stabilizer prepared be provided with excellent thermostability and promote melting, coupling, internal plasticization, the function such as toughness reinforcing, and act synergistically comparatively widely as polyvalent alcohol, hydrotalcite etc. exist with other thermo-stabilizer, PVC thermal stability and processing characteristics can be effectively improved after composite, the preparation method of rare earth thermal stabilizer of the present invention is simple to operate, low in raw material price, provide cost savings, there is great market popularization value.
Embodiment
A preparation method for rare earth thermal stabilizer, comprises the steps:
(1) carboxylic acid, rare earth nitrate salt and sodium hydroxide is taken by amount of substance than 1:1:3;
(2) carboxylic acid, rare earth nitrate salt are dissolved with appropriate dehydrated alcohol and distilled water respectively, disposablely add in three-necked flask, assembling backflow water bath heating device, starts electric stirring;
(3) then sodium hydroxide solution is loaded constant pressure funnel, be slowly added drop-wise in mixing solutions, dropwise rear continuation and react half an hour;
(4) reaction terminates after product vacuum filtration, with dehydrated alcohol and the distilled water wash of heat, dry, obtains white or near-white powder and is product.
The preparation method of a kind of rare earth thermal stabilizer of the present invention, described in step (2), bath temperature is 80 DEG C.Described in step (1), rare earth nitrate salt comprises lanthanum nitrate, cerous nitrate and neodymium nitrate.Described in step (4), the washing times of distilled water is 4 times.Rare-earth carboxylate and calcium stearate/zinc, tetramethylolmethane, hydrotalcite, β – diketone are carried out binary or polynary mixture by certain mass ratio, join in PVC, utilize congo red method to investigate synergy, filter out the formula of the composite thermal stabilizer of stability the best.Then by optimum formula, material is tested processing characteristics on torque rheometer; On open mixing roll, mixing 10 min, dull and stereotyped tabletting machine are pressed into the sheet material of 5mm, utilize the batten needed for universal sampling machine preparation, test mechanical property.Static heat can be made to reach 23min steady time when adding 5 parts of carboxylic acid lanthanums in 100 parts of PVC, sample color is yellow, and relative to the blank sample (3.5 min) of PVC, heat-stable time and tint permanence have had good improvement.Carboxylic acid lanthanum belongs to organic RE type thermal stabilizing agent, according to acid-base principle, and strong acid rare earth ion Re
+with highly basic chlorion Cl unstable in PVC segment
–between there is very strong coordination, can effectively suppress active chlorine remove HCl reaction; In addition, the chlorallylene atom on the replaceable PVC macromole of suitable organic anionic groups, eliminates degraded weakness, reaches thermostable effect.Carboxylic acid lanthanum is carried out binary mixture with tetramethylolmethane, Zinic stearas/calcium, hydrotalcite He β – diketone when mass ratio is 1:1 (totally 5 parts) respectively.Can see that carboxylic acid lanthanum and hydrotalcite, Zinic stearas act synergistically poor, heat-stable time is 14,18 min, is all less than the time of carboxylic acid lanthanum Individual existence, and serious " zinc burning " phenomenon appears in Zinic stearas; Carboxylic acid lanthanum and calcium stearate, β – diketone, tetramethylolmethane exist and act synergistically preferably, heat-stable time is respectively 28,30,37 min, wherein tetramethylolmethane suppresses initial coloration sexuality to be given prominence to, sample about 10 min starts to be colored as light yellow, and 30 min become yellow, and 70 min are brown color.According to above experimental result, determine that carboxylic acid lanthanum and tetramethylolmethane, β – diketone, calcium stearate carry out Recompounded multielement, to improve PVC heat-stable time and to improve tint permanence.Rare earth complex heat stabilizer can promote the plasticizing of PVC better, may be that coordination strong between the chlorine atom in rare earth element and PVC molecule can make the transmission of shearing force be strengthened, thus can promote PVC quick-gelatinizing; Peak torque is suitable with lead salt system with Dynamic Thermal steady time, and balancing torque is higher, and balancing torque temperature is lower.Rare earth element has numerous unoccupied orbitals and larger ionic radius, inorganics in can filling a prescription with PVC and organism form diversified title complex or inner complex, add intermolecular interaction force, physical entanglement point increases, each group partition inter-capacitive strengthens, so that improves intensity and the toughness of material.
Claims (4)
1. a preparation method for rare earth thermal stabilizer, is characterized in that comprising the steps:
(1) carboxylic acid, rare earth nitrate salt and sodium hydroxide is taken by amount of substance than 1:1:3;
(2) carboxylic acid, rare earth nitrate salt are dissolved with appropriate dehydrated alcohol and distilled water respectively, disposablely add in three-necked flask, assembling backflow water bath heating device, starts electric stirring;
(3) then sodium hydroxide solution is loaded constant pressure funnel, be slowly added drop-wise in mixing solutions, dropwise rear continuation and react half an hour;
(4) reaction terminates after product vacuum filtration, with dehydrated alcohol and the distilled water wash of heat, dry, obtains white or near-white powder and is product.
2. the preparation method of a kind of rare earth thermal stabilizer as claimed in claim 1, is characterized in that described in step (2), bath temperature is 80 DEG C.
3. the preparation method of a kind of rare earth thermal stabilizer as claimed in claim 1, is characterized in that described in step (1), rare earth nitrate salt comprises lanthanum nitrate, cerous nitrate and neodymium nitrate.
4. the preparation method of a kind of rare earth thermal stabilizer as claimed in claim 1, is characterized in that the washing times of distilled water described in step (4) is 4 times.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410744121.7A CN104829961A (en) | 2014-12-09 | 2014-12-09 | Preparation method of rare earth thermal-stabilizer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410744121.7A CN104829961A (en) | 2014-12-09 | 2014-12-09 | Preparation method of rare earth thermal-stabilizer |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104829961A true CN104829961A (en) | 2015-08-12 |
Family
ID=53808180
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410744121.7A Pending CN104829961A (en) | 2014-12-09 | 2014-12-09 | Preparation method of rare earth thermal-stabilizer |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104829961A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107090141A (en) * | 2017-04-24 | 2017-08-25 | 内蒙古科技大学 | Pvc heat stabilizer and preparation method thereof |
| CN107602922A (en) * | 2017-08-07 | 2018-01-19 | 郑州庆宏塑胶科技有限公司 | A kind of preparation method of itaconic acid bright-coloured composite thermal stabilizer |
| CN109575470A (en) * | 2018-10-29 | 2019-04-05 | 郭跃 | A kind of preparation method of heat-resistant stable type adhesive protecting film material |
| CN111944253A (en) * | 2020-06-29 | 2020-11-17 | 安徽浩天新型材料有限公司 | Protective tube for automobile wire harness and preparation method thereof |
-
2014
- 2014-12-09 CN CN201410744121.7A patent/CN104829961A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107090141A (en) * | 2017-04-24 | 2017-08-25 | 内蒙古科技大学 | Pvc heat stabilizer and preparation method thereof |
| CN107090141B (en) * | 2017-04-24 | 2019-07-30 | 内蒙古科技大学 | The preparation method of PVC heat stabilizer |
| CN107602922A (en) * | 2017-08-07 | 2018-01-19 | 郑州庆宏塑胶科技有限公司 | A kind of preparation method of itaconic acid bright-coloured composite thermal stabilizer |
| CN109575470A (en) * | 2018-10-29 | 2019-04-05 | 郭跃 | A kind of preparation method of heat-resistant stable type adhesive protecting film material |
| CN111944253A (en) * | 2020-06-29 | 2020-11-17 | 安徽浩天新型材料有限公司 | Protective tube for automobile wire harness and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104829961A (en) | Preparation method of rare earth thermal-stabilizer | |
| CN103194005A (en) | Method for preparing novel polyvinyl chloride (PVC) rare-earth heat stabilizer | |
| CN104804361A (en) | Antibacterial resin composite material and preparation method thereof | |
| CN102675817A (en) | Antibacterial plastic for household appliances and preparation method thereof | |
| CN101717466B (en) | Polyvinyl chloride processing aid and preparation method thereof | |
| CN102627575B (en) | Rare earth complex and its preparation method and use | |
| CN103881199A (en) | Antibacterial antistatic reinforcing master batch used for polyethylene and preparation method thereof | |
| CN102604295B (en) | Polymer calcium zinc complex soap heat stabilizer, preparation method thereof and application thereof | |
| CN104562661A (en) | Cotton and linen fabric finishing process | |
| CN101200556B (en) | Method for synthesizing PVC thermal stabilizer dicarboxylic acids rear earth salt and uses thereof | |
| CN102336985B (en) | Glyceryl calcium/zinc composite heat stabilizer for polyvinyl chloride | |
| CN103483734B (en) | A kind of High-flame-retardancpolyvinyl polyvinyl chloride plastic | |
| CN106243745A (en) | A kind of chlorinated paraffin stabilizer and preparation method thereof | |
| CN104877179A (en) | Organic composite heat stabilizer and preparation method thereof | |
| CN103030906A (en) | Composite plasticizer for polyvinyl chloride | |
| CN105010393A (en) | Preparation method of copper and zinc combination antiseptic | |
| CN103601997A (en) | Polyvinyl chloride plastic with high flame retardance | |
| CN104860281A (en) | Preparation method of aluminum hypophosphite | |
| CN104861393B (en) | A kind of PVC composite thermal stabilizer | |
| CN107793674A (en) | rare earth composite heat stabilizer for PVC and preparation method thereof | |
| CN105647099A (en) | Preparation method of antibacterial ABS resin | |
| CN104946107A (en) | Anti-flaming anti-bacteria coating | |
| CN104327494A (en) | Thermal oxidation stabilizing additive for polyamide | |
| CN107090141B (en) | The preparation method of PVC heat stabilizer | |
| CN105153355A (en) | Preparation method of acrylic resin coating with antibacterial property and light resistance for building |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20150812 |
|
| WD01 | Invention patent application deemed withdrawn after publication |