CN102627575A - Rare earth complex and its preparation method and use - Google Patents
Rare earth complex and its preparation method and use Download PDFInfo
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- CN102627575A CN102627575A CN2012100724729A CN201210072472A CN102627575A CN 102627575 A CN102627575 A CN 102627575A CN 2012100724729 A CN2012100724729 A CN 2012100724729A CN 201210072472 A CN201210072472 A CN 201210072472A CN 102627575 A CN102627575 A CN 102627575A
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Abstract
The invention discloses a rare earth complex. The rare earth complex is an N-alkyl maleamic acid-rare earth complex having a chemical formula of RE(OA)3.nH2O, wherein RE represents a rare-earth element; OA represents N-alkyl maleamic acid radical; and n is equal to 1 or 2. The invention also discloses a preparation method of the rare earth complex and a use of the rare earth complex in a polrvinyl chloride (PVC) heat stabilizer. The rare earth complex can be prepared by simple processes, and has a low cost and industrial application prospects. The rare earth complex or a composition of the rare earth complex as a PVC heat stabilizer overcomes the defects of the existing heat stabilizers, and improves primary dyeing properties and long-term thermal stability of PVC. Especially, the rare earth complex has good synergistic effects with calcium stearate, organic tin and pentaerythritol and thus under unified use, the thermal stability of PVC is improved. In addition, the rare earth complex can effectively improve mechanical properties of a PVC material.
Description
Technical field
The invention belongs to technical field of polymer materials, be specifically related to a kind of rare earth compounding.
Background technology
SE (PVC) plastics are used widely with its good flame retardancy, wear resistance, resistance to chemical corrosion, gas steam low-permeability, comprehensive mechanical performance, the goods transparency, electrical insulating property, sound deadener/insulator etc.Simultaneously, polyvinyl chloride resin also is a kind of thermally sensitive resin, under high temperature and high shear strength, carries out handling ease and sloughs HCl and cause degraded, makes declines such as its product variable color and mechanical property.Therefore in the PVC course of processing, must add certain amount of stabilizer, to improve the decomposition temperature of PVC.Along with the widespread use of hard PVC resin in building trade; The production and consumption total amount of polyvinyl chloride resin will further increase; Thermo-stabilizer is that polyvinyl chloride resin is processed requisite additive; Therefore the production and consumption amount of thermo-stabilizer also will increase gradually, so the development and application of PVC thermo-stabilizer has important economic and social benefit.
The PVC thermo-stabilizer that China uses at present mainly contains 4 big types of lead salt, metallic soap, organotin and rare earth thermal stabilizers etc.The lead salts thermo-stabilizer has remarkable thermostability and cheap price, but the lead salts stablizer is poisonous, lacks oilness, and meets sulphur and can generate black PbS, is unwell to the place that sulphur pollution is arranged.Most of metal soap stabilisers is nontoxic, and certain lubrication is arranged, calcium zinc compound soap particularly, and its use range progressively increases, but there is " zinc burning " problem in calcium zinc heat stabilizer, and relatively poor to the stabilizing power of PVC.The thermal stability of organotin stabilizer is excellent, but it costs an arm and a leg, and current production rate is less.Rare earth class PVC thermo-stabilizer has outstanding thermostability and fast light weathering resistance, unique coupling property, and green, environmental protection, and China is rare earth reserves big countries, therefore develops rare earth thermal stabilizer and has broad prospects in China.
Summary of the invention
Technical problem to be solved by this invention is to above-mentioned deficiency of the prior art, provides a kind of and has outstanding thermostability and fast light weathering resistance and unique coupling property, and rare earth compounding green, environmental protection.
For solving the problems of the technologies described above, the technical scheme that the present invention adopts is: a kind of rare earth compounding, it is characterized in that said rare earth compounding is a N-alkyl maleinamide acid group rare earth compounding, and its chemical molecular formula is R
E(OA)
3NH
2O is in the formula: R
EBe REE, OA is a N-alkyl maleinamide acid group, n=1 or 2; The structural formula of said N-alkyl maleinamide acid group rare earth compounding is:
R is benzyl, allyl group, suitable divinyl methyl, normal hexane base, octyl, decyl, dodecyl, tetradecyl, hexadecyl or octadecyl in the formula.
The present invention also provides the preparation method of above-mentioned rare earth compounding; It is characterized in that; This method is: in N-alkyl maleinamide hydrochlorate ethanolic soln, drip the soluble ree inorganic salt solution while stirring; Be that reaction generates deposition under 20 ℃～50 ℃ the condition in temperature, the washing of precipitate final vacuum is dry, obtain N-alkyl maleinamide acid group rare earth compounding; The mol ratio of said soluble ree inorganic salt and N-alkyl maleinamide hydrochlorate is 1: 2.5～3.5.
Above-mentioned method, the preparation method of said N-alkyl maleinamide hydrochlorate ethanolic soln may further comprise the steps:
Step 1, maleic anhydride and alkylamine mol ratio stirring reaction to the temperature of reaction system in organic solvent according to 1: 1 is begun to descend, it is dry to filter final vacuum, obtains N-alkyl maleinamic acid, and concrete reaction process is following:
Step 2, alkyl maleinamic acid of N-described in the step 1 and alkali are reacted in ethanol, obtain N-alkyl maleinamide hydrochlorate ethanolic soln; The mol ratio of said N-alkyl maleinamic acid and alkali is 1: 1.
Above-mentioned method, organic solvent described in the step 1 are analytically pure ETHYLE ACETATE, ether or acetone.
Above-mentioned method, alkali described in the step 2 are one or more in sodium hydroxide, Pottasium Hydroxide and the ammoniacal liquor, and said ethanol is AR.
Above-mentioned method; Said soluble ree inorganic salt are meant muriate, nitrate salt or the perchlorate of REE, and wherein REE is one or more in scandium, yttrium, lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium and the lutetium.
In addition, the present invention also provides the application of above-mentioned rare earth compounding in polychloroethylene heat stabilizer.
Above-mentioned application, said polychloroethylene heat stabilizer is made up of the raw material of following weight part: 25～100 parts of N-alkyl maleinamide acid group rare earth compoundings, 0～75 part of calcium stearate; 0～12 part of Zinic stearas; 0～10 part of beta-diketon, 0～10 part of tetramethylolmethane, 0～50 part of organotin.
Above-mentioned application, said organotin are dibutyl tin laurate.
Above-mentioned application, the consumption of said polychloroethylene heat stabilizer are 0.5%～3% of SE quality.
The effect evaluation test of rare earth compounding of the present invention in polychloroethylene heat stabilizer:
One, static heat stability test
At first with PVC100 part, 0.5～3 part of N-alkyl maleinamide acid group rare earth compounding thermo-stabilizer or its compsn thermo-stabilizer, 50 parts of DOP (DOP); Mix, place baking oven, 120 ℃ of constant temperature 20min; Make the PVC test piece; Then test piece is cut into the granular sample of about 2mm * 2mm, according to the GB/T2917.1-2002 congo red method: the height of sample in test tube is about 50mm, and the bottom of congo-red test paper is apart from the about 25mm of specimen surface; In 200 ℃ of constant temperature oil baths, the record congo-red test paper occurs significantly being the steady stability time by the blue time of red stain.
Two, dynamically thermal stability test (roller examination method)
With PVC and thermo-stabilizer according to certain mixed evenly after, mixing on 170 ± 3 ℃ rubber mixing machine, the time that the record sample begins blackening, be dynamic heat-stable time.
Three, hot baking method test
With reference to ASTM2115-2004 PVC is tested the sheet sample that print is cut into 1cm * 1cm, place on the aluminium-foil paper, put into 185 ℃ baking oven, every at a distance from 10min sampling observation colour-change situation.Test result shows: the heat-stable time of PVC increases along with the increase of N-alkyl maleinamide acid group rare earth compounding thermo-stabilizer or its compsn thermo-stabilizer consumption; The initial stage thermostability of PVC is progressively improved, and general 2～3 parts N-alkyl maleinamide acid group rare earth compounding thermo-stabilizer or its compsn thermo-stabilizer can satisfy the thermally-stabilised needs to PVC.And the title complex of N-alkyl maleinamide acid group and light rare earths is stronger to the thermally-stabilised ability of PVC.
Four, PVC material properties test
Tensile strength and elongation at break according to GB/T 1040.1-2006 test PVC sample.
Vicat softening point according to GB1633-2000 test plastics.
The present invention compared with prior art has the following advantages:
1, rare earth compounding of the present invention has outstanding thermostability and fast light weathering resistance and unique coupling property, and its preparation method is simple, and green, environmental protection are with low cost, have prospects for commercial application.
2, adopt rare earth compounding of the present invention or its compsn as the PVC thermo-stabilizer; Not only overcome the defective of existing thermo-stabilizer; And elementary tint permanence, long-term thermal stability of making PVC etc. increase; Particularly rare earth compounding and calcium stearate, Zinic stearas, beta-diketon, organotin and tetramethylolmethane etc. have good synergistic, can use the thermal stability that improves PVC jointly.
3, adopt rare earth compounding of the present invention or its compsn as the PVC thermo-stabilizer, can significantly improve the tensile strength and the elongation at break of PVC material, effectively improve the mechanical property of PVC material.
Through embodiment, technical scheme of the present invention is done further detailed description below.
Embodiment
Alkyl in following examples can be with replacing along divinyl methyl, normal hexane base, octyl, decyl, tetradecyl or octadecyl.
Synthetic and the application of the title complex of embodiment 1:N-benzyl maleinamide acid group and lanthanum
Synthetic:
Step 1, with maleic anhydride with etc. refining benzylamine stirring reaction to temperature of reaction system in ETHYLE ACETATE (analytical pure) of amount of substance begin to descend, the filtration final vacuum is dried to constant weight, obtains N-benzyl maleinamic acid;
Step 2, get in the ethanolic soln of sodium hydroxide that the maleinamic acid of N-benzyl described in a certain amount of step 1 joins equimolar amount, obtain the ethanolic soln of N-benzyl maleinamic acid sodium after reacting completely;
Step 3, in the ethanolic soln of the benzyl of N-described in step 2 maleinamic acid sodium, drip stoichiometry (n while stirring
La: n
OA=1: the lanthanum chloride solution of 0.4mol/L 3) is that reaction generated deposition in 20 minutes under 20 ℃ the condition in temperature, sedimentation and filtration is washed final vacuum be dried to constant weight, obtains the title complex of N-benzyl maleinamide acid group and lanthanum.
Through ultimate analysis, infrared spectrum characterization, the chemical constitution of the N-benzyl maleinamide acid group of present embodiment preparation and the title complex of lanthanum is: La (OA)
3H
2O, white or buff powder; Common organic solvents such as water insoluble, ethanol, ether, acetone, and be soluble in N, in N N, the methyl-sulphoxide.
Use:
Test group 1: with PVC 100g, DOP 50g, La (OA)
3H
2O 0.5g mixes, and places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Test group 2: with PVC 100g, DOP 50g, La (OA)
3H
2O 1g mixes, and places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Test group 3: with PVC 100g, DOP 50g, La (OA)
3H
2O 1.5g mixes, and places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Test group 4: with PVC 100g, DOP 50g, La (OA)
3H
2O 2g mixes, and places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Test group 5: with PVC 100g, DOP 50g, La (OA)
3H
2O 2.5g mixes, and places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Control group 1: with PVC 100g, DOP 50g places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Control group 2: with PVC 100g, DOP 50g, the title complex 2.5g of N-phenyl maleimide acid group and lanthanum mixes, and places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Measure static heat steady time (Congo red test), dynamically heat-stable time (roller examination method), the observation of hot baking method respectively.
Table 1 is respectively organized the thermostability comparing result of PVC test piece
Can find out that from table 1 along with the consumption of the title complex of N-benzyl maleinamide acid group and lanthanum increases, all prolong with dynamic heat-stable time static heat steady time of PVC.Compare with the title complex of lanthanum with the N-phenyl maleimide acid group of same amount, adopt static heat steady time and the dynamic heat-stable time equal significant prolongation of the title complex of N-benzyl maleinamide acid group and lanthanum as the PVC of thermo-stabilizer.
With the comparison of other non-toxic stabilizers to the PVC thermostability:
With PVC 100g, DOP 50g, La (OA)
3H
2O or other non-toxic heat stabilizers 2g mix, and place baking oven, in 120 ℃ of constant temperature 20min, make the PVC test piece respectively.Measure static heat steady time (Congo red test), dynamically heat-stable time (roller examination method), the observation of hot baking method respectively, the result is as shown in table 2.Can find out La (OA) from showing interior data
3H
2The thermostability of O stablizer is a little less than organotin stabilizer, and is superior to other non-toxic stabilizers.
Table 2N-benzyl maleinamide acid group and the title complex of lanthanum and the comparison of other hot non-toxic stabilizer
From table 2, can find out, the title complex that adopts N-benzyl maleinamide acid group and lanthanum as static heat steady time of the PVC of thermo-stabilizer and dynamic heat-stable time all apparently higher than other thermo-stabilizers.
The title complex and the calcium stearate of N-benzyl maleinamide acid group and lanthanum have good synergistic, can compositely use.
Control group 1: with PVC 100g, DOP 50g, La (OA)
3H
2O 2.5g mixes, and places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Control group 2: with PVC 100g, DOP 50g, calcium stearate 2.5g mixes, and places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Test group 1: with PVC 100g, DOP 50g, La (OA)
3H
2The mixture 2.5g of O and calcium stearate (mass ratio according to 3: 1 mixes) places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Test group 2: with PVC 100g, DOP 50g, La (OA)
3H
2The mixture 2.5g of O and calcium stearate (mass ratio according to 2: 1 mixes) places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Test group 3: with PVC 100g, DOP 50g, La (OA)
3H
2The mixture 2.5g of O and calcium stearate (mass ratio according to 1: 1 mixes) places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Test group 4: with PVC100g, DOP50g, La (OA)
3H
2The mixture 2.5g of O and calcium stearate (mass ratio according to 1: 2 mixes) places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Test group 5: with PVC100g, DOP50g, La (OA)
3H
2The mixture 2.5g of O and calcium stearate (mass ratio according to 1: 3 mixes) places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Table 3 is respectively organized the thermally-stabilised comparing result of PVC test piece
Synthetic and the application of the title complex of embodiment 2:N-allyl group maleinamide acid group and samarium
Synthetic:
Step 1, with maleic anhydride with etc. refining allyl amine stirring reaction to temperature of reaction system in acetone (analytical pure) of amount of substance begin to descend, the filtration final vacuum is dried to constant weight, obtains N-allyl group maleinamic acid;
Step 2, get in the ethanolic soln of Pottasium Hydroxide that the maleinamic acid of N-allyl group described in a certain amount of step 1 joins equimolar amount, obtain the ethanolic soln of N-allyl group maleinamic acid potassium after reacting completely;
Step 3, in the ethanolic soln of the allyl group of N-described in step 2 maleinamic acid potassium, drip stoichiometry (n while stirring
La: n
OA=1: the samarium nitrate solution of 0.4mol/L 2.5) is that reaction generated deposition in 20 minutes under 30 ℃ the condition in temperature, sedimentation and filtration is washed final vacuum be dried to constant weight, obtains the title complex of N-allyl group maleinamide acid group and samarium.
Through ultimate analysis, infrared spectrum characterization, the chemical constitution of the title complex of product N-allyl group maleinamide acid group and samarium is: S
m(OA)
3H
2O, buff powder; Common organic solvents such as water insoluble, ethanol, ether, acetone, and be soluble in N, in N N, the methyl-sulphoxide.
Use:
Test group 1: with PVC 100g, DOP 50g, S
m(OA)
3H
2O 0.5g mixes, and places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Test group 2: with PVC 100g, DOP 50g, S
m(OA)
3H
2O 1.5g mixes, and places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Test group 3: with PVC 100g, DOP 50g, S
m(OA)
3H
2O 2.5g mixes, and places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Control group 1: with PVC 100g, DOP 50g places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Control group 2: with PVC 100g, DOP 50g, the title complex 2.5g of N-phenyl maleimide acid group and samarium mixes, and places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Measure static heat steady time (Congo red test), dynamically heat-stable time (roller examination method), the observation of hot baking method respectively.
Table 4 is respectively organized the thermostability comparing result of PVC test piece
Can find out that from table 4 along with the consumption of the title complex of N-allyl group maleinamide acid group and samarium increases, all prolong with dynamic heat-stable time static heat steady time of PVC.Compare with the title complex of samarium with the N-phenyl maleimide acid group of same amount, adopt static heat steady time and the dynamic heat-stable time equal significant prolongation of the title complex of N-allyl group maleinamide acid group and samarium as the PVC of thermo-stabilizer.
Synthetic and the application of the title complex of embodiment 3:N-dodecyl maleinamide acid group and dysprosium
Synthetic:
Step 1, with maleic anhydride with etc. refining n-Laurylamine stirring reaction to temperature of reaction system in ether (analytical pure) of amount of substance begin to descend, the filtration final vacuum is dried to constant weight, obtains N-dodecyl maleinamic acid;
Step 2, get in the ethanolic soln of ammoniacal liquor that the maleinamic acid of N-dodecyl described in a certain amount of step 1 joins equimolar amount, obtain N-dodecyl maleinamide hydrochlorate ethanolic soln after reacting completely;
Step 3, in the dodecyl of N-described in step 2 maleinamide hydrochlorate ethanolic soln, drip stoichiometry (n while stirring
La: n
OA=1: the perchloric acid dysprosium solution of 0.4mol/L 3.5) is that reaction generated deposition in 20 minutes under 30 ℃ the condition in temperature, sedimentation and filtration is washed final vacuum be dried to constant weight, obtains the title complex of N-dodecyl maleinamide acid group and dysprosium.
Through ultimate analysis, infrared spectrum characterization, the chemical constitution of the title complex of product N-dodecyl maleinamide acid group and dysprosium is: D
y(OA)
3H
2O, 183 ℃ of fusing points; Common organic solvents such as water insoluble, ethanol, ether, acetone, and be soluble in N, in N N, the methyl-sulphoxide.
Use:
Test group 1: with PVC 100g, DOP 50g, D
y(OA)
3H
2O 0.5g mixes, and places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Test group 2: with PVC 100g, DOP 50g, D
y(OA)
3H
2O 1.5g mixes, and places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Test group 3: with PVC 100g, DOP 50g, D
y(OA)
3H
2O 2.5g mixes, and places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Control group 1: with PVC 100g, DOP 50g places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Control group 2: with PVC 100g, DOP 50g, the title complex 2.5g of N-phenyl maleimide acid group and dysprosium mixes, and places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Measure static heat steady time (Congo red test), dynamically heat-stable time (roller examination method), the observation of hot baking method respectively.
Table 5 is respectively organized the thermostability comparing result of PVC test piece
Can find out that from table 5 along with the consumption of the title complex of N-dodecyl maleinamide acid group and dysprosium increases, all prolong with dynamic heat-stable time static heat steady time of PVC.Compare with the title complex of dysprosium with the N-phenyl maleimide acid group of same amount, adopt static heat steady time and the dynamic heat-stable time equal significant prolongation of the title complex of N-allyl group maleinamide acid group and dysprosium as the PVC of thermo-stabilizer.
Synthetic and the application of the title complex of embodiment 4:N-dodecyl maleinamide acid group and yttrium
Synthetic:
Step 1, with maleic anhydride with etc. refining n-Laurylamine stirring reaction to temperature of reaction system in ETHYLE ACETATE (analytical pure) of amount of substance begin to descend, the filtration final vacuum is dried to constant weight, obtains N-dodecyl maleinamic acid;
Step 2, get in the ethanolic soln of sodium hydroxide that the maleinamic acid of N-dodecyl described in a certain amount of step 1 joins equimolar amount, obtain the ethanolic soln of N-dodecyl maleinamic acid sodium after reacting completely;
Step 3, in the ethanolic soln of the dodecyl of N-described in step 2 maleinamic acid sodium, drip stoichiometry (n while stirring
La: n
OA=1: the yttrium chloride solution of 0.4mol/L 3) is that reaction generated deposition in 10 minutes under 50 ℃ the condition in temperature, sedimentation and filtration is washed final vacuum be dried to constant weight, obtains the title complex of N-dodecyl maleinamide acid group and yttrium.
Through ultimate analysis, infrared spectrum characterization, the chemical constitution of the title complex of product N-dodecyl maleinamide acid group and yttrium is: Y (OA)
32H
2O, white powder; Common organic solvents such as water insoluble, ethanol, ether, acetone, and be soluble in N, in N N, the methyl-sulphoxide.
Use:
Test group 1: with PVC 100g, DOP 50g, Y (OA)
32H
2O 1g mixes, and places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Test group 2: with PVC 100g, DOP 50g, Y (OA)
32H
2O 2g mixes, and places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Test group 3: with PVC 100g, DOP 50g, Y (OA)
32H
2O 3g mixes, and places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Control group 1: with PVC 100g, DOP 50g places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Control group 2: with PVC 100g, DOP 50g, the title complex 3g of N-phenyl maleimide acid group and yttrium mixes, and places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Measure static heat steady time (Congo red test), dynamically heat-stable time (roller examination method), the observation of hot baking method respectively.
Table 6 is respectively organized the thermostability comparing result of PVC test piece
Can find out that from table 6 along with the consumption of the title complex of N-dodecyl maleinamide acid group and yttrium increases, all prolong with dynamic heat-stable time static heat steady time of PVC.Compare with the title complex of yttrium with the N-phenyl maleimide acid group of same amount, adopt static heat steady time and the dynamic heat-stable time equal significant prolongation of the title complex of N-allyl group maleinamide acid group and yttrium as the PVC of thermo-stabilizer.
Synthetic and the application of the title complex of embodiment 5:N-hexadecyl maleinamide acid group and lanthanum
Synthetic:
Step 1, with maleic anhydride with etc. refining cetylamine stirring reaction to temperature of reaction system in ETHYLE ACETATE of amount of substance begin to descend, filter final vacuum and be dried to constant weight, obtain N-hexadecyl maleinamic acid;
Step 2, get in the ethanolic soln of sodium hydroxide that the maleinamic acid of N-hexadecyl described in a certain amount of step 1 joins equimolar amount, obtain N-hexadecyl maleinamide hydrochlorate ethanolic soln after reacting completely;
Step 3, in the hexadecyl of N-described in step 2 maleinamide hydrochlorate ethanolic soln, drip stoichiometry (n while stirring
La: n
OA=1: the lanthanum nitrate hexahydrate of 0.4mol/L 2.5) is that reaction generated deposition in 30 minutes under 25 ℃ the condition in temperature, sedimentation and filtration is washed final vacuum be dried to constant weight, obtains the title complex of N-hexadecyl maleinamide acid group and lanthanum.
Through ultimate analysis, infrared spectrum characterization, the chemical constitution of the title complex of product N-hexadecyl maleinamide acid group and lanthanum is: La (OA)
3H
2O, white or buff powder; Common organic solvents such as water insoluble, ethanol, ether, acetone, and be soluble in N, in N N, the methyl-sulphoxide.
Use:
Test group 1: with PVC 100g, DOP 50g, La (OA)
3H
2O 0.5g mixes, and places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Test group 2: with PVC 100g, DOP 50g, La (OA)
3H
2O 1g mixes, and places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Test group 3: with PVC 100g, DOP 50g, La (OA)
3H
2O 1.5g mixes, and places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Test group 4: with PVC 100g, DOP 50g, La (OA)
3H
2O 2g mixes, and places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Test group 5: with PVC 100g, DOP 50g, La (OA)
3H
2O 2.5g mixes, and places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Control group 1: with PVC 100g, DOP 50g places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Control group 2: with PVC 100g, DOP 50g, the title complex 2.5g of N-phenyl maleimide acid group and lanthanum mixes, and places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Measure static heat steady time (Congo red test), dynamically heat-stable time (roller examination method), the observation of hot baking method respectively.
Table 7 is respectively organized the thermostability comparing result of PVC test piece
Can find out that from table 7 along with the consumption of the title complex of N-hexadecyl maleinamide acid group and lanthanum increases, all prolong with dynamic heat-stable time static heat steady time of PVC.Compare with the title complex of lanthanum with the N-phenyl maleimide acid group of same amount, adopt static heat steady time and the dynamic heat-stable time equal significant prolongation of the title complex of N-hexadecyl maleinamide acid group and lanthanum as the PVC of thermo-stabilizer.
With the comparison of other non-toxic stabilizers to the PVC thermostability:
With PVC 100g, DOP 50g, La (OA)
3H
2O or other non-toxic heat stabilizers 2g mix, and place baking oven, in 120 ℃ of constant temperature 20min, make the PVC test piece respectively.Measure static heat steady time (Congo red test), dynamically heat-stable time (roller examination method), the observation of hot baking method respectively, the result is as shown in table 2.Can find out La (OA) from showing interior data
3H
2The thermostability of O stablizer is a little less than organotin stabilizer, and is superior to other non-toxic stabilizers.
Table 8N-hexadecyl maleinamide acid group and the title complex of lanthanum and the comparison of other hot non-toxic stabilizer
From table 8, can find out, the title complex that adopts hexadecyl maleinamide acid group and lanthanum as static heat steady time of the PVC of thermo-stabilizer and dynamic heat-stable time all apparently higher than other thermo-stabilizers.
N-hexadecyl maleinamide acid group closes lanthanum and calcium stearate has good synergistic, can composite use.
Control group 1: with PVC 100g, DOP 50g, La (OA)
3H
2O 2.5g mixes, and places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Control group 2: with PVC 100g, DOP 50g, calcium stearate 2.5g mixes, and places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Test group 1: with PVC 100g, DOP 50g, La (OA)
3H
2The mixture 2.5g of O and calcium stearate (mass ratio according to 3: 1 mixes) places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Test group 2: with PVC 100g, DOP 50g, La (OA)
3H
2The mixture 2.5g of O and calcium stearate (mass ratio according to 2: 1 mixes) places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Test group 3: with PVC 100g, DOP 50g, La (OA)
3H
2The mixture 2.5g of O and calcium stearate (mass ratio according to 1: 1 mixes) places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Test group 4: with PVC 100g, DOP 50g, La (OA)
3H
2The mixture 2.5g of O and calcium stearate (mass ratio according to 1: 2 mixes) places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Test group 5: with PVC 100g, DOP 50g, La (OA)
3H
2The mixture 2.5g of O and calcium stearate (mass ratio according to 1: 3 mixes) places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Table 9 N-hexadecyl maleinamide acid group close lanthanum with
The composite use of calcium stearate is to the thermostable effect of PVC
Synthetic and the application of the title complex of embodiment 6:N-hexadecyl maleinamide acid group and samarium
Synthetic:
Step 1, with maleic anhydride with etc. refining cetylamine stirring reaction to temperature of reaction system in ether (analytical pure) of amount of substance begin to descend, the filtration final vacuum is dried to constant weight, obtains N-hexadecyl maleinamic acid;
Step 2, get in the ethanolic soln of sodium hydroxide and Pottasium Hydroxide that the maleinamic acid of N-hexadecyl described in a certain amount of step 1 joins equimolar amount, obtain N-hexadecyl maleinamide hydrochlorate ethanolic soln after reacting completely;
Step 3, in the hexadecyl of N-described in step 2 maleinamide hydrochlorate ethanolic soln, drip stoichiometry (n while stirring
La: n
OA=1: the samarium trichloride solution of 0.4mol/L 3) is that reaction generated deposition in 30 minutes under 25 ℃ the condition in temperature, sedimentation and filtration is washed final vacuum be dried to constant weight, obtains the title complex of N-hexadecyl maleinamide acid group and samarium.
Through ultimate analysis, infrared spectrum characterization, the chemical constitution of the title complex of product N-hexadecyl maleinamide acid group and samarium is: S
m(OA)
3H
2O, buff powder; Common organic solvents such as water insoluble, ethanol, ether, acetone, and be soluble in N, in N N, the methyl-sulphoxide.
Use:
Test group 1: with PVC 100g, DOP 50g, S
m(OA)
3H
2O 0.5g mixes, and places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Test group 2: with PVC 100g, DOP 50g, S
m(OA)
3H
2O 1.5g mixes, and places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Test group 3: with PVC 100g, DOP 50g, S
m(OA)
3H
2O 2.5g mixes, and places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Control group 1: with PVC 100g, DOP 50g places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Control group 2: with PVC 100g, DOP 50g, the title complex 2.5g of N-phenyl maleimide acid group and samarium mixes, and places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.Measure static heat steady time (Congo red test), dynamically heat-stable time (roller examination method), the observation of hot baking method respectively.
Table 10 is respectively organized the thermostability comparing result of PVC test piece
Can find out that from table 10 along with the consumption of the title complex of N-hexadecyl maleinamide acid group and samarium increases, all prolong with dynamic heat-stable time static heat steady time of PVC.Compare with the title complex of samarium with the N-phenyl maleimide acid group of same amount, adopt static heat steady time and the dynamic heat-stable time equal significant prolongation of the title complex of N-hexadecyl maleinamide acid group and samarium as the PVC of thermo-stabilizer.
Synthetic and the application of the title complex of embodiment 7:N-hexadecyl maleinamide acid group and dysprosium
Synthetic:
Step 1, with maleic anhydride with etc. refining cetylamine stirring reaction to temperature of reaction system in ETHYLE ACETATE (analytical pure) of amount of substance begin to descend, the filtration final vacuum is dried to constant weight, obtains N-hexadecyl maleinamic acid;
Step 2, get in the ethanolic soln of sodium hydroxide and ammoniacal liquor that the maleinamic acid of N-hexadecyl described in a certain amount of step 1 joins equimolar amount, obtain N-hexadecyl maleinamide hydrochlorate ethanolic soln after reacting completely;
Step 3, in the hexadecyl of N-described in step 2 maleinamide hydrochlorate ethanolic soln, drip stoichiometry (n while stirring
La: n
OA=1: the Dysprosium trichloride solution of 0.4mol/L 3) is that reaction generated deposition in 20 minutes under 20 ℃ the condition in temperature, sedimentation and filtration is washed final vacuum be dried to constant weight, obtains the title complex of N-hexadecyl maleinamide acid group and dysprosium.
Through ultimate analysis, infrared spectrum characterization, the chemical constitution of the title complex of product N-hexadecyl maleinamide acid group and dysprosium is: D
y(OA)
3H
2O, 183 ℃ of fusing points; Common organic solvents such as water insoluble, ethanol, ether, acetone, and be soluble in N, in N N, the methyl-sulphoxide.
Use:
Test group 1: with PVC 100g, DOP 50g, D
y(OA)
3H
2O 0.5g mixes, and places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Test group 2: with PVC 100g, DOP 50g, D
y(OA)
3H
2O 1.5g mixes, and places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Test group 3: with PVC 100g, DOP 50g, D
y(OA)
3H
2O 2.5g mixes, and places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Control group 1: with PVC 100g, DOP 50g places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Control group 2: with PVC 100g, DOP 50g, the title complex 2.5g of N-phenyl maleimide acid group and dysprosium mixes, and places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Measure static heat steady time (Congo red test), dynamically heat-stable time (roller examination method), the observation of hot baking method respectively.
Table 11 is respectively organized the thermostability comparing result of PVC test piece
Can find out that from table 11 along with the consumption of the title complex of N-hexadecyl maleinamide acid group and dysprosium increases, all prolong with dynamic heat-stable time static heat steady time of PVC.Compare with the title complex of dysprosium with the N-phenyl maleimide acid group of same amount, adopt static heat steady time and the dynamic heat-stable time equal significant prolongation of the title complex of N-hexadecyl maleinamide acid group and dysprosium as the PVC of thermo-stabilizer.
Synthetic and the application of the title complex of embodiment 8:N-hexadecyl maleinamide acid group and yttrium
Synthetic:
Step 1, with maleic anhydride with etc. refining cetylamine stirring reaction to temperature of reaction system in acetone (analytical pure) of amount of substance begin to descend, the filtration final vacuum is dried to constant weight, obtains N-hexadecyl maleinamic acid;
Step 2, get in the ethanolic soln of sodium hydroxide that the maleinamic acid of N-hexadecyl described in a certain amount of step 1 joins equimolar amount, obtain the ethanolic soln of N-hexadecyl maleinamic acid sodium after reacting completely;
Step 3, in the ethanolic soln of the hexadecyl of N-described in step 2 maleinamic acid sodium, drip stoichiometry (n while stirring
La: n
OA=1: the yttrium chloride solution of 0.4mol/L 3) is that reaction generated deposition in 20 minutes under 20 ℃ the condition in temperature, sedimentation and filtration is washed final vacuum be dried to constant weight, obtains the title complex of N-hexadecyl maleinamide acid group and yttrium.
Through ultimate analysis, infrared spectrum characterization, the chemical constitution of the title complex of product N-hexadecyl maleinamide acid group and yttrium is: Y (OA)
32H
2O, white powder; Common organic solvents such as water insoluble, ethanol, ether, acetone, and be soluble in N, in N N, the methyl-sulphoxide.
Use:
Test group 1: with PVC 100g, DOP 50g, Y (OA)
32H
2O 1g mixes, and places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Test group 2: with PVC 100g, DOP 50g, Y (OA)
32H
2O 2g mixes, and places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Test group 3: with PVC 100g, DOP 50g, Y (OA)
32H
2O 3g mixes, and places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Control group 1: with PVC 100g, DOP 50g places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Control group 2: with PVC 100g, DOP 50g, the title complex 3g of N-phenyl maleimide acid group and yttrium mixes, and places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Measure static heat steady time (Congo red test), dynamically heat-stable time (roller examination method), the observation of hot baking method respectively.
Table 12 is respectively organized the thermostability comparing result of PVC test piece
Can find out that from table 12 along with the consumption of the title complex of N-hexadecyl maleinamide acid group and yttrium increases, all prolong with dynamic heat-stable time static heat steady time of PVC.Compare with the title complex of yttrium with the N-phenyl maleimide acid group of same amount, adopt static heat steady time and the dynamic heat-stable time equal significant prolongation of the title complex of N-hexadecyl maleinamide acid group and yttrium as the PVC of thermo-stabilizer.
Synthetic and the application of embodiment 9:N-hexadecyl maleinamide acid group and light rare earths mixed ligand complex:
Synthetic:
Step 1, with maleic anhydride with etc. refining cetylamine stirring reaction to temperature of reaction system in ETHYLE ACETATE (analytical pure) of amount of substance begin to descend, the filtration final vacuum is dried to constant weight, obtains N-hexadecyl maleinamic acid;
Step 2, get in the ethanolic soln of sodium hydroxide that the maleinamic acid of N-hexadecyl described in a certain amount of step 1 joins equimolar amount, obtain the ethanolic soln of N-hexadecyl maleinamic acid sodium after reacting completely;
Step 3, commercially available light rare earths mixed chloride is made into the R of 0.4mol/L
E 3+Solution is regulated pH with aqueous sodium hydroxide solution and is about about 6, does not have deposition and generates; In the ethanolic soln of the hexadecyl of N-described in step 2 maleinamic acid sodium, drip stoichiometry (n while stirring
RE: n
OA=1: R 3)
E 3+Solution is that reaction generated deposition in 30 minutes under 25 ℃ the condition in temperature, sedimentation and filtration is washed final vacuum be dried to constant weight, obtains N-hexadecyl maleinamide acid group and light rare earths mixed ligand complex.
Through ultimate analysis, infrared spectrum characterization, the chemical constitution of product N-hexadecyl maleinamide acid group and light rare earths mixed ligand complex is: R
E(OA)
3H
2O, micro-yellow powder, common organic solvents such as water insoluble, ethanol, ether, acetone, and be soluble in N, in N N, the methyl-sulphoxide.
Use:
Test group 1: with PVC 100g, DOP 50g, R
E(OA)
3H
2O 0.5g mixes, and places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Test group 2: with PVC 100g, DOP 50g, R
E(OA)
3H
2O 1.5g mixes, and places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Test group 3: with PVC 100g, DOP 50g, R
E(OA)
3H
2O 2.5g mixes, and places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Control group 1: with PVC 100g, DOP 50g places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Control group 2: with PVC100g, DOP50g, N-phenyl maleimide acid group and light rare earths mixed ligand complex 2.5g mix, and place baking oven, in 120 ℃ of constant temperature 20min, make the PVC test piece.
Measure static heat steady time (Congo red test), dynamically heat-stable time (roller examination method), the observation of hot baking method respectively.
Table 13 is respectively organized the thermostability comparing result of PVC test piece
Can find out that from table 13 along with the consumption increase of N-hexadecyl maleinamide acid group and light rare earths mixed ligand complex, the static heat of PVC all prolongs with dynamic heat-stable time steady time.Compare with the light rare earths mixed ligand complex with the N-phenyl maleimide acid group of same amount, adopt N-hexadecyl maleinamide acid group and light rare earths mixed ligand complex static heat steady time and the dynamic equal significant prolongation of heat-stable time as the PVC of thermo-stabilizer.
Embodiment 10: the effect of combination PVC thermo-stabilizer
Control group 1: with PVC 100g, DOP 50g places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Control group 2: with PVC 100g, DOP 50g, commercially available calcium zinc stabilizer 2.5g mixes, and places baking oven, in 120 ℃ of constant temperature 20min, makes the PVC test piece.
Control group 3: with PVC 100g; DOP 50g; Combination PVC thermo-stabilizer 2.5g (title complex of N-phenyl maleimide acid group and lanthanum, calcium stearate and tetramethylolmethane are according to the mixed uniformly mixture of 45: 45: 10 mass ratio) mixes; Place baking oven,, make the PVC test piece in 120 ℃ of constant temperature 20min.
Test group 1: with PVC 100g, DOP 50g, combination PVC thermo-stabilizer 2.5g (La (OA)
3H
2O, calcium stearate and tetramethylolmethane are according to the mixed uniformly mixture of 45: 45: 10 mass ratio) mix, place baking oven, in 120 ℃ of constant temperature 20min, make the PVC test piece.
Test group 2: with PVC 100g, DOP 50g, combination PVC thermo-stabilizer 2.5g (D
y(OA)
3H
2O, calcium stearate and beta-diketon are according to the mixed uniformly mixture of 47: 47: 10 mass ratio) mix, place baking oven, in 120 ℃ of constant temperature 20min, make the PVC test piece.
Test group 3: with PVC 100g, DOP 50g, combination PVC thermo-stabilizer 2.5g (S
m(OA)
3H
2O, calcium stearate, Zinic stearas and tetramethylolmethane were according to 42: 42: 12: the mixed uniformly mixture of 4 mass ratio) mix, place baking oven, in 120 ℃ of constant temperature 20min, make the PVC test piece.
Test group 4: with PVC 100g, DOP 50g, combination PVC thermo-stabilizer 2.5g (Y (OA)
3H
2O, calcium stearate, Zinic stearas and tetramethylolmethane were according to 42: 42: 12: the mixed uniformly mixture of 4 mass ratio) mix, place baking oven, in 120 ℃ of constant temperature 20min, make the PVC test piece.
Test group 5: with PVC 100g, DOP 50g, combination PVC thermo-stabilizer 2.5g (N-alkyl maleinamide acid group and light rare earths mixed ligand complex RE
(OA)
3H
2O, calcium stearate, Zinic stearas and tetramethylolmethane were according to 22: 66: 8: the mixed uniformly mixture of 4 mass ratio) mix, place baking oven, in 120 ℃ of constant temperature 20min, make the PVC test piece.
Test group 6: with PVC 100g, DOP 50g, combination PVC thermo-stabilizer 2.5g (N-hexadecyl maleinamide acid group and light rare earths mixed ligand complex R
E(OA)
3H
2O and organotin-dibutyl tin laurate are according to the mixed uniformly mixture of 50: 50 mass ratio) mix, place baking oven, in 120 ℃ of constant temperature 20min, make the PVC test piece.
Measure static heat steady time (Congo red test), dynamically heat-stable time (roller examination method), the observation of hot baking method respectively.
Table 14 combination PVC thermo-stabilizer is to the thermostability contrast of PVC
Embodiment 11: the effect of different thermo-stabilizers
With PVC 200g, thermo-stabilizer 6g, calcium stearate 1.4g, Triple Pressed Stearic Acid 1.2g, CaCO
320g, TiO
24g mixes, and 175 ℃ two rolls melting mixing on the plasticator, mixes rear tab and takes off, and on vulcanizing press, carries out mold pressing, and molding temperature is that 175 ℃, molding pressure are 10MPa; Fully fusion and keep 3min after carry out the pressurize cooling, dwell pressure is 7MPa, in the time of 60 ℃, take out, according to the standard sample preparation, the evaluating material performance.
Comparative group 1: thermo-stabilizer is organotin-dibutyl tin laurate.
Comparative group 2: thermo-stabilizer is a complex lead salt stabilizer.
Comparative group 3: thermo-stabilizer is the title complex of N-phenyl maleimide acid group and lanthanum.
Test group 1: thermo-stabilizer is N-dodecyl maleinamide acid group and light rare earths mixed ligand complex.
Test group 2: thermo-stabilizer is the title complex of N-benzyl maleinamide acid group and lanthanum.
Test group 3: thermo-stabilizer is combination PVC thermo-stabilizer (S
m(OA)
3H
2O, calcium stearate, Zinic stearas and tetramethylolmethane were according to 42: 42: 12: the mixed uniformly mixture of 4 mass ratio).
Test group 4: thermo-stabilizer is combination PVC thermo-stabilizer (N-hexadecyl maleinamide acid group and light rare earths mixed ligand complex R
E(OA)
3H
2O calcium stearate, Zinic stearas and tetramethylolmethane were according to 22: 66: 8: the mixed uniformly mixture of 4 mass ratio).
Test group 5: thermo-stabilizer is: combination PVC thermo-stabilizer 6 (N-hexadecyl maleinamide acid group and light rare earths mixed ligand complex R
E(OA)
3H
2O, organotin-dibutyl tin laurate are according to the mixed uniformly mixture of 50: 50 mass ratio).
Table 15 adopts the PVC performance comparison result of different stabilizers
From table 15, can find out; Adopt rare earth compounding of the present invention or its compsn as the PVC thermo-stabilizer; Tensile strength and elongation at break to the PVC material all are improved to some extent, and explain that rare earth compounding of the present invention or its compsn thermo-stabilizer can effectively improve the mechanical property of PVC material.
In sum; Adopt rare earth compounding of the present invention or its compsn as the PVC thermo-stabilizer; Not only overcome the defective of existing thermo-stabilizer; And the elementary tint permanence, long-term thermal stability etc. of PVC are increased, particularly N-alkyl maleinamide acid group rare earth compounding and calcium stearate, organotin, tetramethylolmethane etc. have good synergistic, can use the thermal stability that improves PVC jointly; In addition, rare earth compounding of the present invention or its compsn thermo-stabilizer can effectively improve the mechanical property of PVC material.
The above; It only is preferred embodiment of the present invention; Be not that the present invention is done any restriction, every technical spirit changes any simple modification, change and the equivalence that above embodiment did according to the present invention, all still belongs in the protection domain of technical scheme of the present invention.
Claims (10)
1. a rare earth compounding is characterized in that, said rare earth compounding is a N-alkyl maleinamide acid group rare earth compounding, and its chemical molecular formula is R
E(OA)
3NH
2O is in the formula: R
EBe REE, OA is a N-alkyl maleinamide acid group, n=1 or 2; The structural formula of said N-alkyl maleinamide acid group rare earth compounding is:
R is benzyl, allyl group, suitable divinyl methyl, normal hexane base, octyl, decyl, dodecyl, tetradecyl, hexadecyl or octadecyl in the formula.
2. one kind prepares the method for rare earth compounding according to claim 1; It is characterized in that; This method is: in N-alkyl maleinamide hydrochlorate ethanolic soln, drip the soluble ree inorganic salt solution while stirring; Be that reaction generates deposition under 20 ℃～50 ℃ the condition in temperature, the washing of precipitate final vacuum is dry, obtain N-alkyl maleinamide acid group rare earth compounding; The mol ratio of said soluble ree inorganic salt and N-alkyl maleinamide hydrochlorate is 1: 2.5～3.5.
3. method according to claim 2 is characterized in that, the preparation method of said N-alkyl maleinamide hydrochlorate ethanolic soln may further comprise the steps:
Step 1, maleic anhydride and alkylamine mol ratio stirring reaction to the temperature of reaction system in organic solvent according to 1: 1 is begun to descend, it is dry to filter final vacuum, obtains N-alkyl maleinamic acid, and concrete reaction process is following:
Step 2, alkyl maleinamic acid of N-described in the step 1 and alkali are reacted in ethanol, obtain N-alkyl maleinamide hydrochlorate ethanolic soln; The mol ratio of said N-alkyl maleinamic acid and alkali is 1: 1.
4. method according to claim 3 is characterized in that, organic solvent described in the step 1 is analytically pure ETHYLE ACETATE, ether or acetone.
5. method according to claim 3 is characterized in that, alkali described in the step 2 is one or more in sodium hydroxide, Pottasium Hydroxide and the ammoniacal liquor, and said ethanol is AR.
6. method according to claim 2; It is characterized in that; Said soluble ree inorganic salt are meant muriate, nitrate salt or the perchlorate of REE, and wherein REE is one or more in scandium, yttrium, lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium and the lutetium.
7. the application of rare earth compounding in polychloroethylene heat stabilizer according to claim 1.
8. application according to claim 7; It is characterized in that said polychloroethylene heat stabilizer is made up of the raw material of following weight part: 25～100 parts of N-alkyl maleinamide acid group rare earth compoundings, 0～75 part of calcium stearate; 0～12 part of Zinic stearas; 0～10 part of beta-diketon, 0～10 part of tetramethylolmethane, 0～50 part of organotin.
9. application according to claim 8 is characterized in that, said organotin is a dibutyl tin laurate.
10. application according to claim 8 is characterized in that, the consumption of said polychloroethylene heat stabilizer is 0.5%～3% of a SE quality.
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