JPH0374681B2 - - Google Patents
Info
- Publication number
- JPH0374681B2 JPH0374681B2 JP61121280A JP12128086A JPH0374681B2 JP H0374681 B2 JPH0374681 B2 JP H0374681B2 JP 61121280 A JP61121280 A JP 61121280A JP 12128086 A JP12128086 A JP 12128086A JP H0374681 B2 JPH0374681 B2 JP H0374681B2
- Authority
- JP
- Japan
- Prior art keywords
- vent
- section
- volatile substances
- water
- resin
- 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.)
- Expired - Lifetime
Links
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 35
- 239000000126 substance Substances 0.000 claims description 28
- 229920000642 polymer Polymers 0.000 claims description 18
- 229920003002 synthetic resin Polymers 0.000 claims description 9
- 239000000057 synthetic resin Substances 0.000 claims description 9
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 6
- 229920005989 resin Polymers 0.000 description 16
- 239000011347 resin Substances 0.000 description 16
- 238000001125 extrusion Methods 0.000 description 8
- 238000002347 injection Methods 0.000 description 8
- 239000007924 injection Substances 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 229920000122 acrylonitrile butadiene styrene Polymers 0.000 description 4
- 230000006835 compression Effects 0.000 description 4
- 238000007906 compression Methods 0.000 description 4
- XECAHXYUAAWDEL-UHFFFAOYSA-N acrylonitrile butadiene styrene Chemical compound C=CC=C.C=CC#N.C=CC1=CC=CC=C1 XECAHXYUAAWDEL-UHFFFAOYSA-N 0.000 description 3
- 239000004676 acrylonitrile butadiene styrene Substances 0.000 description 3
- 238000013022 venting Methods 0.000 description 3
- 238000012662 bulk polymerization Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005187 foaming Methods 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 239000004793 Polystyrene Substances 0.000 description 1
- 238000010793 Steam injection (oil industry) Methods 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 229920006026 co-polymeric resin Polymers 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000007720 emulsion polymerization reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 238000010528 free radical solution polymerization reaction Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229920005669 high impact polystyrene Polymers 0.000 description 1
- 239000004797 high-impact polystyrene Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 229920002285 poly(styrene-co-acrylonitrile) Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001256 steam distillation Methods 0.000 description 1
- 229920003048 styrene butadiene rubber Polymers 0.000 description 1
- 238000004781 supercooling Methods 0.000 description 1
- 238000010557 suspension polymerization reaction Methods 0.000 description 1
Landscapes
- Graft Or Block Polymers (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明はスチレン系合成樹脂から、その樹脂中
に含有されている揮発性物質を除去する方法に関
するものである。DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a method for removing volatile substances contained in a styrenic synthetic resin.
最近、スチレン系合成樹脂は自動車部品、家庭
電化製品、玩具、食品容器等広範囲の用途で使用
されている。この原料樹脂中に未反応単量体およ
び溶媒などの揮発性物質が残留すると、樹脂製品
の機械的性質、耐熱性などの熱的性質または耐薬
品性などの化学的性質を低下させることがよく知
られている。
Recently, styrene-based synthetic resins have been used in a wide range of applications such as automobile parts, home appliances, toys, and food containers. If volatile substances such as unreacted monomers and solvents remain in this raw resin, they often deteriorate the mechanical properties, thermal properties such as heat resistance, or chemical properties such as chemical resistance of the resin product. Are known.
また樹脂成形時に、これらの揮発性物質が揮散
し成形加工作業環境を悪化させる。 Furthermore, during resin molding, these volatile substances evaporate and deteriorate the molding work environment.
これらの点からスチレン系合成樹脂中の揮発性
物質を効率的に除去し、残留揮発性物質含有量を
低下させることが技術課題となつている。 From these points of view, it has become a technical issue to efficiently remove volatile substances from styrenic synthetic resins and reduce the content of residual volatile substances.
一方、スチレン系合成樹脂の揮発性物質除去方
法として、特公昭52−31271号公報に記載されて
いるようにベント式押出機を用い、ベント部前に
水またはスチームを注入し、ベント部を減圧下に
保持することが提案されている。 On the other hand, as a method for removing volatile substances from styrenic synthetic resins, as described in Japanese Patent Publication No. 52-31271, a vent type extruder is used, water or steam is injected in front of the vent part, and the pressure is reduced in the vent part. It is suggested to keep it below.
しかし、水注入の場合には押出機の押出能力を
増大させると、注入した水の発泡によるサージン
グなどの押出・吐出不安定性を生ずる。また水注
入部でポリマの過冷却を生じ、ポリマの溶融粘度
が異常上昇し、ポリマのベントアツプにより真空
ベント部が閉塞し、生産を再三中断することにな
り、生産効率を低下させる。 However, in the case of water injection, increasing the extrusion capacity of the extruder causes extrusion/discharge instability such as surging due to foaming of the injected water. Furthermore, supercooling of the polymer occurs in the water injection section, the melt viscosity of the polymer increases abnormally, and the vacuum vent section is clogged due to the venting of the polymer, resulting in repeated interruptions of production and lowering production efficiency.
更に、水蒸気注入の場合には、押出機内での樹
脂の発泡が激しく、押出能力が低下するととも
に、定常的な樹脂の吐出が困難となり、ベントア
ツプの頻度が激しく、生産を再三中断し、生産効
率を低下させることもある。 Furthermore, in the case of steam injection, the resin foams violently in the extruder, reducing extrusion capacity and making it difficult to discharge resin regularly, resulting in frequent vent-ups, which repeatedly interrupts production and reduces production efficiency. It may also reduce the
そこで本発明者らは、前記欠点を克服すべく鋭
意研究したところ、スチレン系合成樹脂から揮発
性物質をベント式押出機にて効率的に除去し、残
留揮発性物質の含有量を著しく低下する方法を見
出した。
Therefore, the present inventors conducted intensive research to overcome the above-mentioned drawbacks, and found that volatile substances can be efficiently removed from styrenic synthetic resin using a vented extruder, and the content of residual volatile substances can be significantly reduced. I found a way.
本発明は、スチレン系溶融ポリマから揮発性物
質を除去するに際し、ベント式押出機を使用し、
ベント前のバレル部に120℃以上の加圧加熱水を
１ベント当り、押出ポリマ通過量の0.5重量％以
上注入し、ベント部圧力を300mmHg（絶対圧）以
下に保持する方法である。
The present invention uses a vented extruder to remove volatile substances from a molten styrenic polymer,
This is a method in which pressurized heated water at 120°C or higher is injected into the barrel section before the vent, at least 0.5% by weight of the amount of extruded polymer passing through each vent, and the pressure at the vent section is maintained at 300 mmHg (absolute pressure) or less.
本発明を適用し得るスチレン系合成樹脂は、汎
用ポリスチレン、耐衝撃性ポリスチレン、ABS
樹脂、スチレン−アクリロニトリル共重合体、ス
チレン−ブタジエン共重合体等があり、これらの
合成樹脂を製造する方法としては塊状重合、溶液
重合、懸濁重合、乳化重合などの製造法のいずれ
でもよい。 Styrenic synthetic resins to which the present invention can be applied include general-purpose polystyrene, high-impact polystyrene, and ABS.
There are resins, styrene-acrylonitrile copolymers, styrene-butadiene copolymers, etc., and methods for producing these synthetic resins include bulk polymerization, solution polymerization, suspension polymerization, and emulsion polymerization.
例えば、塊状重合設備からスチレン系合成樹脂
を溶融状態でベント式押出機に直接供給し、揮発
性物質を除去するプロセスにも適用できる。 For example, it can be applied to a process in which styrenic synthetic resin is directly fed in a molten state from bulk polymerization equipment to a vented extruder to remove volatile substances.
押出機内に注入する加圧加熱水は、120℃以上、
好ましくは120〜250℃、更に好ましくは145〜170
℃である。この温度が120℃以下ならば、サージ
ング、ベントアツプが生じ好ましくない。また、
加圧加熱水は重合体の品質劣化および押出機に使
用されている材料への悪影響を与える物質を含有
していないことが好ましく、加圧加熱した純水が
最も良い。 The pressurized heated water injected into the extruder must be at a temperature of 120℃ or higher,
Preferably 120-250℃, more preferably 145-170
It is ℃. If this temperature is below 120°C, surging and venting may occur, which is undesirable. Also,
It is preferable that the pressurized and heated water does not contain substances that would deteriorate the quality of the polymer or adversely affect the materials used in the extruder, and pure water that has been pressurized and heated is best.
また加圧加熱水は、水の水蒸気圧以上、通常30
〜60Kg／cm2・Ｇ、最大65Kg／cm2・Ｇで使用する。 In addition, pressurized heated water has a pressure higher than the water vapor pressure of water, usually 30
~60Kg/ cm2・G, maximum 65Kg/ cm2・G.
注入する加圧加熱水の量は、１ベント当り押出
ポリマ通過量0.5重量％以上、好ましくは２〜10
重量％、更に好ましくは２〜５重量％であり、押
出機タイプ、ポリマ温度、樹脂の溶融粘度等を考
慮し、最適の注水量を選定することになる。0.5
重量％以下ならば揮発性物質の除去を十分できな
いため、水蒸気蒸溜が十分達成できない。また、
この量が多過ぎるとベントアツプが起り易いため
好ましくない。 The amount of pressurized heated water to be injected is 0.5% by weight or more, preferably 2 to 10% by weight of extruded polymer passing through per vent.
% by weight, more preferably 2 to 5% by weight, and the optimum amount of water to be poured should be selected in consideration of the extruder type, polymer temperature, melt viscosity of the resin, etc. 0.5
If it is less than % by weight, volatile substances cannot be removed sufficiently and steam distillation cannot be achieved satisfactorily. Also,
If this amount is too large, vent-up is likely to occur, which is undesirable.
本発明にて使用される押出機は単軸または２軸
で、ベント部を１ヶ所以上有し、加圧加熱水の注
入ヶ所は１ヶ所以上の複数ヶ所であつてもよい。
加圧加熱水の注入装置としては、例えば定量容積
式加圧ポンプ（プランジヤポンプ）にて純水を数
十気圧に加圧後、２重管式加熱器でそのジヤケツ
ト側をスチームにて120℃以上に加熱することに
よつて達成できる。 The extruder used in the present invention may be a single-screw or twin-screw extruder, and may have one or more vents, and the pressurized and heated water may be injected at one or more locations.
As an injection device for pressurized heated water, for example, after pressurizing pure water to several tens of atmospheres using a fixed displacement pressure pump (plunger pump), the jacket side is heated to 120°C with steam using a double pipe heater. This can be achieved by heating to a higher temperature.
またベント部における真空度は300mmHg（絶対
圧）以下、好ましくは30〜300ｍHgとする。多段
ベント式押出機においては、１段ベント部の真空
度を200mmHg（絶対圧）以下、２段ベント部以降
を100mmHg（絶対圧）以下とするのが好ましい。 Further, the degree of vacuum in the vent section is 300 mmHg (absolute pressure) or less, preferably 30 to 300 mHg. In a multi-stage vent type extruder, it is preferable that the degree of vacuum in the first stage vent part be 200 mmHg (absolute pressure) or less, and in the second stage vent part and onward to 100 mmHg (absolute pressure) or less.
本発明の作用を第１図のベント式押出機概念図
をもつて説明する。
The operation of the present invention will be explained with reference to the conceptual diagram of a vent type extruder shown in FIG.
スチレン系溶融樹脂またはペレツトを樹脂供給
口１より供給し、単軸または２軸の押出スクリユ
ー７にて加熱溶融圧縮する。 Molten styrene resin or pellets are supplied from the resin supply port 1 and heated, melted and compressed by a single or twin screw extrusion screw 7.
ポリマ供給圧縮部（Ａ部）に定量加圧ポンプに
て、注入水を水注入バレル部４のポリマ圧力以上
の圧力に保持し、120℃以上に加熱した加圧加熱
水を加圧加熱水注入口２より注入する。 The injection water is maintained at a pressure higher than the polymer pressure in the water injection barrel section 4 using a constant pressure pump in the polymer supply compression section (section A), and the pressurized heated water heated to 120°C or higher is injected into the polymer supply compression section (section A). Inject from inlet 2.
注入された加圧加熱水は、ベント部（Ｄ部）に
おいてスクリユーの剪断混合作用で溶融ポリマと
均一混合され、ベント部圧力300mmHg以下の圧力
に保持することによつて、ポリマ中の揮発性物質
とともにベント孔３から除去される。揮発性物質
と水が除去されたポリマはスクリユ計量部で圧縮
定量され、ダイス部６より吐出される。 The injected pressurized heated water is uniformly mixed with the molten polymer by the shear mixing action of the screw in the vent section (D section), and by maintaining the pressure at the vent section pressure at 300 mmHg or less, volatile substances in the polymer are removed. At the same time, it is removed from the vent hole 3. The polymer from which volatile substances and water have been removed is compressed and quantified in the screw metering section, and then discharged from the die section 6.
本発明を実施例、比較例でもつて説明する。 The present invention will be explained with reference to Examples and Comparative Examples.
２軸のベント式押出機を用い、ABS（アクリロ
ニトリル−ブタジエン−スチレン共重合）樹脂の
揮発性物質除去試験を行なつた。 A test for removing volatile substances from ABS (acrylonitrile-butadiene-styrene copolymer) resin was conducted using a twin-screw vented extruder.
使用したベント式押出機は第１図に示されると
おりであり、軸径が60mmφ、Ｌ／Ｄ＝32で、ベン
ト部前のバレル部４に加熱加圧水の注入口を設け
た（Ｄ部）。 The vent type extruder used was as shown in FIG. 1, with a shaft diameter of 60 mmφ, L/D=32, and an injection port for heated and pressurized water was provided in the barrel section 4 in front of the vent section (section D).
試験に供したABS樹脂中には揮発性物質が
3500ppm存在し、樹脂供給孔１から押出機内に供
給した。供給された樹脂は、供給圧縮部（Ａ部）
で溶融される。溶融樹脂流れに対し加圧加熱水注
入口２より所定量の加熱水をプランジヤポンプに
てポリマ中に注入する。 There were volatile substances in the ABS resin used in the test.
It was present at 3500 ppm and was supplied into the extruder through resin supply hole 1. The supplied resin is transferred to the supply compression section (A section)
It is melted in A predetermined amount of heated water is injected into the polymer from the pressurized heated water inlet 2 using a plunger pump against the flow of the molten resin.
注入された水はベント孔３にて300mmHg以下の
圧力に保持され、揮発性物質とともに排気され、
樹脂中の揮発性物質が除去される。揮発性物質が
除去された樹脂は計量部（Ｂ部）で加圧され、ヘ
ツドダイ部（Ｃ部）より押出しされる。 The injected water is maintained at a pressure of 300 mmHg or less at vent hole 3, and is exhausted together with volatile substances.
Volatile substances in the resin are removed. The resin from which volatile substances have been removed is pressurized in the measuring section (section B) and extruded from the head die section (section C).
試験結果を表１に示す。 The test results are shown in Table 1.
実施例１〜５では注入水量0.5％以上、注入水
温120〜150℃、注入水圧力35〜43Kg／cm2Ｇ、ベン
ト真空度100〜300mmHg（絶対圧）で樹脂中の揮発
性物質含有量を0.1％以下に減少させることがで
き、押出時のサージング、ベントアツプもなく押
出量も203〜208Kg／Hrと運転状態は安定してい
た。 In Examples 1 to 5, the volatile substance content in the resin was determined at an injected water amount of 0.5% or more, an injected water temperature of 120 to 150°C, an injected water pressure of 35 to 43 Kg/cm 2 G, and a vent vacuum of 100 to 300 mmHg (absolute pressure). The operating conditions were stable, with no surging or venting during extrusion, and the extrusion rate was 203 to 208 kg/hr.
これに対し比較例６、７、10は注入水温がそれ
ぞれ30℃、80℃と120℃以下であるため、押出時
にサージングを生じ運転状態が不安定であつた。
比較例８では注入水量が0.3％と低く、揮発性物
質含有量を0.1％以下にすることができなかつた。
比較例９にて加圧加熱水のかわりに４Kg／cm2Ｇの
飽和水蒸気を注入したところ、ベント部での発泡
が激しく、ベントアツプを生じ、生産継続が困難
であつた。比較例11においては、ベント真空度が
350mmHgとなり、揮発性物質含有量を0.1％以下
にすることができなかつた。 On the other hand, in Comparative Examples 6, 7, and 10, the injection water temperatures were 30° C., 80° C., and 120° C. or lower, respectively, so surging occurred during extrusion, resulting in unstable operating conditions.
In Comparative Example 8, the amount of water injected was as low as 0.3%, and the volatile substance content could not be reduced to 0.1% or less.
In Comparative Example 9, when 4 kg/cm 2 G of saturated steam was injected instead of pressurized and heated water, foaming at the vent part was severe, causing vent up-up, making it difficult to continue production. In Comparative Example 11, the degree of vent vacuum was
350mmHg, making it impossible to reduce the volatile substance content to 0.1% or less.
本発明ではベント部前のバレル部に加圧加熱水
を注入し、ベント部の圧力を低くすることによ
り、スチレン系溶融ポリマから揮発性物質を効率
良く0.1％以下にすることができる。しかも、こ
の揮発性物質の除去は、押出時のサージング、ベ
ントアツプ等のトラブルもなく、安定した運転状
態で行なうことができる。
In the present invention, by injecting pressurized heated water into the barrel section in front of the vent section and lowering the pressure at the vent section, volatile substances can be efficiently reduced to 0.1% or less from the molten styrene polymer. Moreover, this removal of volatile substances can be carried out under stable operating conditions without any troubles such as surging or vent-up during extrusion.
第１図は本発明の実施態様を示すためのベント
式押出機概形図である。
１は樹脂供給口、２は加圧加熱水注入口、３は
ベント孔、４はバレル部、５は押出機ヘツド、６
はダイス部、７は単軸または２軸スクリユーを示
す。Ａ部は供給圧縮部、Ｂ部は計量部、Ｃ部はヘ
ツドダイ部、Ｄ部は加圧加熱水注入部／ベント部
を示す。
FIG. 1 is a schematic diagram of a vent-type extruder showing an embodiment of the present invention. 1 is a resin supply port, 2 is a pressurized heated water inlet, 3 is a vent hole, 4 is a barrel part, 5 is an extruder head, 6
7 indicates a die portion, and 7 indicates a single or double screw. Part A is a supply compression part, part B is a metering part, part C is a head die part, and part D is a pressurized and heated water injection part/vent part.
Claims (1)
するに際し、ベント式押出機を使用し、ベント部
前のバレル部に120℃以上の加圧加熱水を１ベン
ト当り、押出ポリマ通過量の0.5重量％以上注入
し、ベント部圧力を300mmHg（絶対圧）以下に保
持することを特徴とするスチレン系合成樹脂より
揮発性物質を除去する方法。1. When removing volatile substances from molten styrenic polymer, use a vent-type extruder and pour pressurized heated water at 120°C or higher into the barrel in front of the vent for each vent, at 0.5% by weight of the amount of extruded polymer passing through. A method for removing volatile substances from styrene-based synthetic resin, characterized by injecting the above amount and maintaining the vent pressure at 300 mmHg (absolute pressure) or less.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP12128086A JPS62280205A (en) | 1986-05-28 | 1986-05-28 | Removal of volatile matter from styrenic synthetic resin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP12128086A JPS62280205A (en) | 1986-05-28 | 1986-05-28 | Removal of volatile matter from styrenic synthetic resin |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS62280205A JPS62280205A (en) | 1987-12-05 |
| JPH0374681B2 true JPH0374681B2 (en) | 1991-11-27 |
Family
ID=14807345
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP12128086A Granted JPS62280205A (en) | 1986-05-28 | 1986-05-28 | Removal of volatile matter from styrenic synthetic resin |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS62280205A (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0356504A (en) * | 1989-07-26 | 1991-03-12 | Idemitsu Petrochem Co Ltd | Method for removing residual volatile content of styrenic polymer |
| AU2001286250A1 (en) * | 2000-09-14 | 2002-03-26 | Jsp Corporation | Core material for vacuum heat insulation material and vacuum heat insulation material |
| EP1671772A1 (en) * | 2003-08-28 | 2006-06-21 | Tadahiro Ohmi | Apparatus for producing polymer |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60231750A (en) * | 1984-05-02 | 1985-11-18 | Japan Synthetic Rubber Co Ltd | Thermoplastic resin composition |
-
1986
- 1986-05-28 JP JP12128086A patent/JPS62280205A/en active Granted
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60231750A (en) * | 1984-05-02 | 1985-11-18 | Japan Synthetic Rubber Co Ltd | Thermoplastic resin composition |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS62280205A (en) | 1987-12-05 |
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