CN101525402B - Preparation method of maleic anhydride graft polybutylene succinate (PBS) alloy - Google Patents

Preparation method of maleic anhydride graft polybutylene succinate (PBS) alloy Download PDF

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CN101525402B
CN101525402B CN2009101062396A CN200910106239A CN101525402B CN 101525402 B CN101525402 B CN 101525402B CN 2009101062396 A CN2009101062396 A CN 2009101062396A CN 200910106239 A CN200910106239 A CN 200910106239A CN 101525402 B CN101525402 B CN 101525402B
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maleic anhydride
pbs
parts
alloy
heating
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CN101525402A (en
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尹建伟
居学成
刘勇
余汉成
刘钊
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SHENZHEN WEIMING BEIKE ENVIRONMENTAL MATERIAL CO., LTD.
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SHENGANG MANUFACTURE-LEARNING-RESEARCH BASE INDUSTRY DEVELOPMENT CENTER
SHENZHEN WEIMING-PKU BIOMATERIALS Co Ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/88—Thermal treatment of the stream of extruded material, e.g. cooling
    • B29C48/919—Thermal treatment of the stream of extruded material, e.g. cooling using a bath, e.g. extruding into an open bath to coagulate or cool the material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
    • B29C48/04—Particle-shaped
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
    • B29C48/395—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders
    • B29C48/40—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders using two or more parallel screws or at least two parallel non-intermeshing screws, e.g. twin screw extruders
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/88—Thermal treatment of the stream of extruded material, e.g. cooling
    • B29C48/918—Thermal treatment of the stream of extruded material, e.g. cooling characterized by differential heating or cooling
    • B29C48/9185—Thermal treatment of the stream of extruded material, e.g. cooling characterized by differential heating or cooling in the direction of the stream of the material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/92—Measuring, controlling or regulating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92504—Controlled parameter
    • B29C2948/92561—Time, e.g. start, termination, duration or interruption
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92504—Controlled parameter
    • B29C2948/92704—Temperature
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92819—Location or phase of control
    • B29C2948/92857—Extrusion unit
    • B29C2948/92876—Feeding, melting, plasticising or pumping zones, e.g. the melt itself
    • B29C2948/92895—Barrel or housing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92819—Location or phase of control
    • B29C2948/92857—Extrusion unit
    • B29C2948/92904—Die; Nozzle zone

Abstract

The invention relates to a maleic anhydride graft polybutylene succinate (PBS) alloy, comprising the following ingredients in terms of the weight ratios: 100 parts of PBS, 20-30 parts of polylactic resin, 1.0-2.0 parts of maleic anhydride monomer, 0.02-0.05 part of initiator and 0.4-1.0 part of acetone. The degradable materials formed by the maleic anhydride monomer graft PBS and polylactic acid having excellent mechanical property, tensile strength and elongation at break; each material system has better compatibility. The invention also relates to a method for preparing the alloy material.

Description

The manufacture method of maleic anhydride graft polybutylene succinate (PBS) alloy
[technical field]
The present invention relates to a kind of degradable material and manufacture method thereof, especially relate to a kind of manufacture method of maleic anhydride graft polybutylene succinate (PBS) alloy.
[background technology]
Along with the usage quantity of electric equipment products is increasing, it is also more and more to scrap electric equipment products, and the objectionable impurities in these wastes causes very big harm to environment and human health.Can effectively address these problems with biodegradable material.
Poly butylene succinate (PBS) enters the investigation of materials field the nineties in 20th century, but and become one of the focus material of the universal complete biodegradable plastics research of wide popularization and application rapidly, compare characteristics such as that PBS has is cheap, mechanical property excellence with polycaprolactone (PCL), poly butyric ester (PHB), poly hydroxy acid degradative plasticss such as (PHA); And compare with the poly(lactic acid) (PLA) of close prices, it is easy to process that PBS has again, can adapt to the plastic processing of present routine, the characteristics that resistance toheat is good, and its heat-drawn wire can surpass 88 ℃ (heat resisting temperature of PLA has only about 60 ℃).And PBS synthetic raw material sources both can be petroleum resources, also can obtain by the biomass resource fermentation, had therefore caused showing great attention to of science and technology and industrial community.In these aliphatic polyesters that can degrade fully, PBS becomes present one of the universal degradative plastics of industrialization prospect that has most.
PBS is formed through polycondensation by Succinic Acid and butyleneglycol, density 1.26g/cm3, and 114 ℃ of fusing points, different according to the height of molecular weight and molecular weight distribution, degree of crystallinity is 30%～45%.
But PBS also has significant disadvantages: melt strength is low in the course of processing; The moulded products physical and mechanical properties is low;
And because of the melt strength of PBS and PLA, degree of crystallinity etc. differed far away, the direct comixing compatibility of two-phase is relatively poor.
[summary of the invention]
In view of this, be necessary to provide a kind of maleic anhydride graft polybutylene succinate (PBS) alloy.Have better consistency by each material system in the degradable material that poly butylene succinate is carried out graft modification, make obtaining, and have excellent mechanical property, tensile strength and elongation at break simultaneously.
A kind of method for preparing maleic anhydride graft polybutylene succinate (PBS) alloy may further comprise the steps: raw-material pre-treatment, poly butylene succinate, polylactic resin are sloughed surperficial steam by vacuum drying tank; Poly butylene succinate, polylactic resin, maleic anhydride, initiator, acetone etc. are measured by following part by weight, and add the mixing of stirrer high speed: 100 parts of poly butylene succinates, 20～30 parts of polylactic resin, 1.0～2.0 parts of maleic anhydride monomers, 0.02～0.05 part of initiator, 0.4～1.0 part in acetone; In double screw rod extruder, carry out reactive grafting, and the traction, tie rod, granulation under water.
By maleic anhydride graft polybutylene succinate (PBS)/poly(lactic acid) system, make each material system in the degradable material that obtains have better consistency, and possess excellent mechanical property, tensile strength and elongation at break simultaneously.
In a preferred embodiment, the number-average molecular weight of described poly butylene succinate is 100,000 to 200,000.Preferred poly butylene succinate can be taken into account the physical strength and the toughness of degradable material.
In a preferred embodiment, the weight-average molecular weight of described polylactic resin is 50,000 to 400,000.The fluidity of molten of preferred poly(lactic acid) is better.
In a preferred embodiment, the purity of described maleic anhydride monomer is the chemical pure level.Adopt highly purified maleic anhydride monomer can guarantee the unicity of grafted monomer, thereby guarantee the performance of degradable material
In a preferred embodiment, described initiator is the benzoyl peroxide of analytical pure level.Because the dosage of initiator is considerably less, adopts analytically pure benzoyl peroxide can guarantee the effect of initiator in graft reaction.
Wherein, each of described double screw rod extruder section temperature is set as follows: 110～120 ℃ of charging openings, 120～130 ℃ in one district of heating, 130～140 ℃ in two districts of heating, 140～150 ℃ in three districts of heating, heat four districts 150～160 ℃, heat 160～165 ℃ in five districts, 160～170 ℃ of head temperatures.
Wherein, the reaction time of material in double screw rod extruder is less than 40s, and vacuum tightness is-0.08MPa.
[embodiment]
Be further detailed below in conjunction with specific embodiment.
The present invention relates to a kind of maleic anhydride graft polybutylene succinate (PBS) alloy, component that it comprises and weight proportion are: 100 parts of poly butylene succinates; 20～30 parts of polylactic resin; 1.0～2.0 parts of maleic anhydride monomers; 0.02～0.05 part of initiator; 0.4～1.0 part in acetone.
Its preparation process is as follows:
Poly butylene succinate, polylactic resin are sloughed surperficial steam by vacuum drying tank;
Poly butylene succinate, polylactic resin, maleic anhydride, initiator, acetone etc. are measured by above-mentioned part by weight, and add the mixing of stirrer high speed;
In double screw rod extruder, carry out reactive grafting, and the traction, tie rod, granulation under water.
The double screw rod extruder parameter setting is as follows:
Figure DEST_PATH_RE-GSB00000256293100031
The feeding manner that adopts is hungry feeding, prevents that feeding is too fast, overflow occurs.
The reaction time of material in double screw rod extruder is less than 40s.
Embodiment 1
Get 100 parts of poly butylene succinates by weight, 20 parts of polylactic resin, 1.0 parts of maleic anhydrides, 0.02 part of initiator, 0.4 part in acetone;
Poly butylene succinate, polylactic resin are sloughed surperficial steam by vacuum drying tank;
Poly butylene succinate, polylactic resin, maleic anhydride, initiator, acetone are added stirrer for mixing;
According to the condition of the double screw rod extruder of above-mentioned setting, mixed material is dropped into double screw rod extruder carry out reactive grafting, and traction, tie rod, granulation under water.
Embodiment 2
Get 100 parts of poly butylene succinates by weight, 20 parts of polylactic resin, 2.0 parts of maleic anhydrides, 0.05 part of initiator, 1.0 parts in acetone.
Identical among other steps and the embodiment 1.
Embodiment 3
Get 100 parts of poly butylene succinates by weight, 30 parts of polylactic resin, 1.0 parts of maleic anhydrides, 0.02 part of initiator, 0.4 part in acetone.
Identical among other steps and the embodiment 1.
Embodiment 4
Get 100 parts of poly butylene succinates by weight, 30 parts of polylactic resin, 2.0 parts of maleic anhydrides, 0.05 part of initiator, 1.0 parts in acetone.
Identical among other steps and the embodiment 1.
The degradable material salient features that each embodiment obtains sees the following form:
Test subject Unit Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4
The Izod notched Izod impact strength ?KJ/m2? ?＞30KJ/m2? ?＞30KJ/m2? ?＞30KJ/m2? ?＞30KJ/m2?
Elongation at break ?％? ?＞20? ?＞20? ?＞20? ?＞20?
Tensile strength ?MPa? ?＞35? ?＞35? ?＞35? ?＞35?
The RoHs instruction Up to standard Up to standard Up to standard Up to standard Up to standard
Biodegradable Up to standard Up to standard Up to standard Up to standard Up to standard
As can be seen from the above table, maleic anhydride graft polybutylene succinate (PBS) alloy material of the present invention, the physical and mechanical properties height, intensity is big, and shock resistance is good, and is biodegradable.
The above embodiment has only expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to claim of the present invention.Should be pointed out that for the person of ordinary skill of the art without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.

Claims (3)

1. the manufacture method of a maleic anhydride graft polybutylene succinate (PBS) alloy is characterized in that, may further comprise the steps:
Raw-material pre-treatment is sloughed surperficial steam with poly butylene succinate, polylactic resin by vacuum drying tank;
Poly butylene succinate, polylactic resin, maleic anhydride, initiator, acetone are measured by following part by weight, and add the mixing of stirrer high speed: 100 parts of poly butylene succinates, 20～30 parts of polylactic resin, 1.0～2.0 parts of maleic anhydride monomers, 0.02～0.05 part of initiator, 0.4～1.0 part in acetone; The number-average molecular weight of described poly butylene succinate is 100,000 to 200,000, and the weight-average molecular weight of described polylactic resin is 50,000 to 400,000;
In double screw rod extruder, carry out reactive grafting, and the traction, tie rod, granulation under water, each of described double screw rod extruder section temperature is set as follows: 110～120 ℃ of charging openings, 120～130 ℃ in one district of heating, 130～140 ℃ in two districts of heating, 140～150 ℃ in three districts of heating, 150～160 ℃ in four districts of heating, 160～165 ℃ in five districts of heating, 160～170 ℃ of head temperatures, and the reaction time of material in double screw rod extruder is less than 40s, and vacuum tightness is-0.08MPa.
2. the manufacture method of maleic anhydride graft polybutylene succinate (PBS) alloy as claimed in claim 1 is characterized in that, described maleic anhydride monomer purity is the chemical pure level.
3. the manufacture method of maleic anhydride graft polybutylene succinate (PBS) alloy as claimed in claim 1 is characterized in that, described initiator is the benzoyl peroxide of analytical pure level.
CN2009101062396A 2009-03-27 2009-03-27 Preparation method of maleic anhydride graft polybutylene succinate (PBS) alloy Expired - Fee Related CN101525402B (en)

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CN102276846B (en) * 2011-05-31 2013-02-20 中国科学院长春应用化学研究所 Modified poly lactic acid, and preparation method thereof
CN104231512A (en) * 2014-08-27 2014-12-24 广东红旗家具有限公司 Preparation method of degradable wood-plastic composite material and degradable wood-plastic composite material
CN104530669B (en) * 2014-12-18 2017-10-03 陈梓煜 It is a kind of for modified polylactic acid material of 3D printing and preparation method thereof
CN105400117B (en) * 2015-11-23 2019-12-13 厦门理工学院 anti-droplet expansion flame-retardant poly (butylene succinate) and preparation method thereof
CN105440602B (en) * 2015-12-23 2017-08-08 山东国塑科技实业有限公司 Coir fibre/poly butylene succinate composite and preparation method thereof
US11898032B2 (en) * 2018-09-07 2024-02-13 Chien-Chung Huang Biodegradable composition
CN110527269B (en) * 2019-09-02 2021-10-01 福建鑫邦新材料科技有限公司 Modified polycarbonate material and preparation method thereof
CN114014987A (en) * 2021-12-02 2022-02-08 北京大学深圳研究院 Degradable composite biological high polymer material and preparation method thereof

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