JPH04246423A - Method for preventing resin from blocking in reaction tank - Google Patents
Method for preventing resin from blocking in reaction tankInfo
- Publication number
- JPH04246423A JPH04246423A JP1012891A JP1012891A JPH04246423A JP H04246423 A JPH04246423 A JP H04246423A JP 1012891 A JP1012891 A JP 1012891A JP 1012891 A JP1012891 A JP 1012891A JP H04246423 A JPH04246423 A JP H04246423A
- Authority
- JP
- Japan
- Prior art keywords
- resin
- reaction tank
- tank
- reaction
- water
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 45
- 229920005989 resin Polymers 0.000 title claims abstract description 40
- 239000011347 resin Substances 0.000 title claims abstract description 40
- 230000000903 blocking effect Effects 0.000 title claims abstract description 9
- 238000000034 method Methods 0.000 title claims description 11
- 238000003756 stirring Methods 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000012295 chemical reaction liquid Substances 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- 238000005507 spraying Methods 0.000 claims description 2
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 abstract description 8
- 238000004140 cleaning Methods 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 238000000151 deposition Methods 0.000 abstract 1
- 238000012423 maintenance Methods 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- 239000007788 liquid Substances 0.000 description 11
- 238000000605 extraction Methods 0.000 description 7
- 239000002002 slurry Substances 0.000 description 6
- 239000000243 solution Substances 0.000 description 5
- 239000004372 Polyvinyl alcohol Substances 0.000 description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 description 4
- 230000002194 synthesizing effect Effects 0.000 description 4
- 238000011001 backwashing Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- ZTQSAGDEMFDKMZ-UHFFFAOYSA-N Butyraldehyde Chemical compound CCCC=O ZTQSAGDEMFDKMZ-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical group CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 1
- 239000003377 acid catalyst Substances 0.000 description 1
- 239000004840 adhesive resin Substances 0.000 description 1
- 229920006223 adhesive resin Polymers 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 229920002689 polyvinyl acetate Polymers 0.000 description 1
- 239000011118 polyvinyl acetate Substances 0.000 description 1
- 238000011027 product recovery Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- HGBOYTHUEUWSSQ-UHFFFAOYSA-N valeric aldehyde Natural products CCCCC=O HGBOYTHUEUWSSQ-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
- Polymerisation Methods In General (AREA)
Abstract
Description
【0001】0001
【産業上の利用分野】この発明は、反応槽内でポリビニ
ルブチラールなどのように合着しやすい樹脂を合成する
際に樹脂が反応槽中でブロック化するのを防止する方法
に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention This invention relates to a method for preventing resins from forming blocks in a reaction tank when synthesizing resins that tend to coalesce, such as polyvinyl butyral.
【0002】0002
【従来の技術】一般に、合成樹脂は、反応槽に原材料を
投入し、触媒等の働きによって原材料を重合や縮合させ
ることにより得られるようになっている。たとえば、可
塑剤を加えることによって、自着性に優れた合わせガラ
ス用中間膜を形成するポリビニルブチラール(以下、「
PVB」と記す)は、酸触媒の存在下に水の入った反応
槽内にポリビニルアルコールとブチルアルデヒドとを入
れ撹拌しつつ反応(縮合反応)させる等することにより
得られるようになっている。2. Description of the Related Art Generally, synthetic resins are obtained by charging raw materials into a reaction tank and polymerizing or condensing the raw materials under the action of a catalyst or the like. For example, by adding a plasticizer, polyvinyl butyral (hereinafter referred to as "
PVB) can be obtained by placing polyvinyl alcohol and butyraldehyde in a reaction tank containing water in the presence of an acid catalyst and reacting (condensation reaction) with stirring.
【0003】0003
【発明が解決しようとする課題】ところで、上記のよう
にして樹脂を合成する場合、通常、反応中の反応液の温
度を一定にするために、反応槽を囲むように設けられた
ジャケットによって一定温度になるように加熱されてい
る。したがって、反応槽の液界面上部の槽壁および撹拌
機の撹拌軸等が乾燥しており、液界面から飛散した樹脂
スラリーがこれらにあたると瞬時に乾燥し硬化してしま
う。そして、硬化した付着樹脂が界面で何重にも重なり
巨大なフィルム状付着物となる。この付着物は自重や撹
拌による液流などにより剥離して反応液中に落ちたりす
ることがあるが、PVBなどの合着しやすい樹脂の場合
は、この落下した付着物が液中で撹拌されているうちに
、樹脂をも取り込み巨大なブロックとなってしまう。
したがって、反応が終了し、反応槽の下部に設けられた
下部抜出口からスラリー状の樹脂を抜き出す時に、ブロ
ックが下部抜出口が詰まってしまい、抜き出しに時間が
かかるばかりか、逆洗いなどの余分な作業も行わなけれ
ばならない。特に巨大なブロックは、逆洗いなどをして
も下部抜出口から落下しないため、人手によって反応槽
の上部マンホールから掻き上げて取り出すようにしてお
り、工数がかかり危険であるとともに、製品の歩留まり
も悪いものである。また、槽壁に付着した付着物は、反
応が終了するごとに高圧水やヘラを用いて洗浄するよう
にしているが、洗浄により槽壁を傷めて槽の寿命が短く
なったり、槽壁の滑らかさが損なわれるため、次の反応
時に付着が促進すると言う問題がある。さらに、硬化が
ひどければ、人が槽内に入って除去作業を行わなければ
ならず、手間がかかるとともに、危険であると言う問題
もあった。この発明は、このような事情に鑑みて、製品
の回収率を向上させるとともに、槽の清掃作業やブロッ
クの除去作業などを軽減させる等、生産効率を向上でき
る反応槽における樹脂のブロック化防止方法を提供する
ことを目的としている。[Problems to be Solved by the Invention] When synthesizing a resin as described above, normally, in order to keep the temperature of the reaction solution constant during the reaction, a jacket is provided surrounding the reaction tank to keep the temperature constant. heated to a certain temperature. Therefore, the tank wall above the liquid interface of the reaction tank, the stirring shaft of the stirrer, etc. are dry, and when the resin slurry scattered from the liquid interface hits these, it instantly dries and hardens. Then, the hardened adhesive resin overlaps many layers at the interface to form a huge film-like deposit. This deposit may peel off due to its own weight or the liquid flow caused by stirring and fall into the reaction solution, but in the case of resins that tend to coalesce, such as PVB, this fallen deposit may be stirred in the liquid. While it is being used, it also absorbs resin and becomes a huge block. Therefore, when the reaction is finished and the slurry-like resin is extracted from the lower outlet provided at the bottom of the reaction tank, the block clogs the lower outlet, which not only takes time but also requires extra time such as backwashing. work must also be done. In particular, huge blocks do not fall out of the lower extraction port even after backwashing, so they have to be manually scraped up and removed from the upper manhole of the reaction tank, which is time-consuming and dangerous, and also reduces product yield. It's bad. In addition, deposits on the tank walls are cleaned using high-pressure water or a spatula after each reaction, but cleaning may damage the tank walls and shorten the life of the tank. Since the smoothness is impaired, there is a problem that adhesion is promoted during the next reaction. Furthermore, if the hardening is severe, a person has to enter the tank to remove it, which is both time-consuming and dangerous. In view of these circumstances, this invention provides a method for preventing resin from forming blocks in a reaction tank, which can improve production efficiency by improving product recovery rate, reducing tank cleaning work, block removal work, etc. is intended to provide.
【0004】0004
【課題を解決するための手段】この発明は、このような
目的を達成するために、反応槽内で原料となる物質を反
応させて所望の樹脂を合成する際に反応液中での樹脂の
ブロック化を防止する方法であって、反応中、液界面近
傍部およびその上方部の反応槽内壁面および撹拌機の撹
拌軸に散水して撹拌等により飛散した反応液中の樹脂の
付着を防止することを特徴とする反応槽内における樹脂
のブロック化防止方法を要旨としている。[Means for Solving the Problems] In order to achieve the above-mentioned object, the present invention aims to reduce the amount of resin in the reaction solution when synthesizing a desired resin by reacting raw materials in a reaction tank. This is a method to prevent blocking, and during the reaction, water is sprinkled on the inner wall surface of the reaction tank near the liquid interface and above it, as well as on the stirring shaft of the stirrer, to prevent the adhesion of resin in the reaction liquid that is scattered due to stirring, etc. The gist of this paper is a method for preventing resin blocking in a reaction tank, which is characterized by:
【0005】[0005]
【作用】上記構成によれば、反応槽の液界面近傍部およ
びその上方部の槽内壁面および撹拌機の撹拌軸に反応中
に散水することにより、槽内壁面および撹拌機の撹拌軸
へ飛散した樹脂スラリーを樹脂が硬化して付着する前に
洗い流して槽内に戻すようにできる。[Operation] According to the above structure, by spraying water on the tank inner wall surface near the liquid interface of the reaction tank and above it, and on the stirring shaft of the stirrer during the reaction, water is scattered onto the inner wall surface of the tank and the stirring shaft of the stirrer. The resin slurry can be washed away and returned to the tank before the resin hardens and adheres.
【0006】[0006]
【実施例】以下に、この発明を、その実施例をあらわす
図面を参照しつつ詳しく説明する。この発明にかかる反
応槽における樹脂のブロック化防止方法を実施するのに
は、特に限定されないが、たとえば、図1にみるような
装置を用いることができる。この装置は、図にみるよう
に、反応槽1がジャケット6で覆われているとともに反
応槽1内部に撹拌翼2、散水リング7やバッフル3を備
えている。撹拌翼2はその撹拌軸21の回転により反応
槽1内部の反応液を撹拌するようになっていて、特に限
定されないが、ファウドラー翼を用いることが好ましい
。散水リング7は、注水口8から注水されることにより
反応液界面近傍部およびその上方部の槽内壁面11およ
び撹拌翼2の撹拌軸21に散水するようになっている。
図中、4は上部マンホール、5は下部抜出口である。つ
ぎに、この装置を用いた実施例を比較例とあわせて説明
する。DESCRIPTION OF THE PREFERRED EMBODIMENTS The present invention will be explained in detail below with reference to the drawings showing embodiments thereof. To carry out the method of preventing resin blocking in a reaction tank according to the present invention, for example, an apparatus as shown in FIG. 1 can be used, although there is no particular limitation. As shown in the figure, this device includes a reaction tank 1 covered with a jacket 6, and a stirring blade 2, a water sprinkling ring 7, and a baffle 3 inside the reaction tank 1. The stirring blade 2 is configured to stir the reaction liquid inside the reaction tank 1 by rotating the stirring shaft 21, and is preferably a Faudler blade, although it is not particularly limited. The water sprinkling ring 7 is configured to spray water onto the tank inner wall surface 11 in the vicinity of the reaction liquid interface and above the reaction liquid interface and on the stirring shaft 21 of the stirring blade 2 by injecting water from the water injection port 8 . In the figure, 4 is an upper manhole, and 5 is a lower outlet. Next, examples using this device will be described together with comparative examples.
【0007】(実施例1)反応槽1にPVB樹脂を合成
する原料を仕込み、100rpm の回転速度で撹拌翼
2を回転させて撹拌しながら加熱用ジャケット6に蒸気
(7kgG/cm2 、140℃)を通し、反応槽1内
の温度を70℃まで昇温したのち、撹拌しながら5時間
放置した。また、反応中、散水リング7から20℃の水
を槽内壁面11および撹拌軸21へ散水し続けた。散水
総量は反応槽1中の全液量の5%(3.5l/min)
であった。そして、5時間経過後に得られた反応槽1内
のPVB樹脂スラリーを下部抜出口5から抜き出したと
ころ、ブロック量は全樹脂量の1.5 %で、かつ、全
体的に小さいものばかりで、全て良好に抜き出すことが
できた。また、液界面近傍部およびその上方部の槽内壁
面11およひ撹拌軸21への樹脂の付着はほとんどなく
、抜き出し後槽壁に付着した樹脂は、散水リング7から
散水するとすべて洗い流せた。その付着量は全樹脂量の
1.3 %であった。(Example 1) Raw materials for synthesizing PVB resin are charged into a reaction tank 1, and steam (7 kgG/cm2, 140°C) is supplied to a heating jacket 6 while stirring by rotating the stirring blade 2 at a rotational speed of 100 rpm. The temperature inside the reaction tank 1 was raised to 70° C., and then left for 5 hours with stirring. Further, during the reaction, water at 20° C. was continuously sprayed from the water sprinkling ring 7 onto the tank inner wall surface 11 and the stirring shaft 21. The total amount of water sprinkled is 5% of the total amount of liquid in reaction tank 1 (3.5 l/min)
Met. When the PVB resin slurry in the reaction tank 1 obtained after 5 hours was extracted from the lower extraction port 5, the amount of blocks was 1.5% of the total amount of resin, and the blocks were generally small. I was able to extract everything successfully. Further, there was almost no resin adhering to the tank inner wall surface 11 and stirring shaft 21 in the vicinity of the liquid interface and above it, and all the resin adhering to the tank wall after extraction was washed away by sprinkling water from the water sprinkling ring 7. The adhesion amount was 1.3% of the total resin amount.
【0008】(比較例1)散水しなかった以外は実施例
1と同様にしてPVB樹脂スラリーを得た。得られたP
VB樹脂スラリーを下部抜出口5から抜き出したところ
直径10cm程度のブロックがたくさんあり、抜き出し
作業中に、下部抜出口5が何度も閉塞し、逆洗などの作
業を行わなければならず多大な時間を要した。また、下
部抜出口5の径より大きいブロックもあり、このような
巨大なブロックは、人手により上部マンホール4から掻
き出さなければならなかった。なお、ブロック量は、全
樹脂量の9.1 %であった。しかも、液界面近傍部の
槽内壁面11に樹脂の付着物が厚さ1〜3cm、幅40
cmで全周にわたってリング状に付着しており、散水リ
ング7から散水を行ったが取れなかった。付着量は全樹
脂量の4.2 %であった。(Comparative Example 1) A PVB resin slurry was obtained in the same manner as in Example 1 except that water was not sprinkled. Obtained P
When the VB resin slurry was extracted from the lower outlet 5, there were many blocks with a diameter of about 10 cm, and during the extraction process, the lower outlet 5 was blocked many times, requiring backwashing and other work. It took time. Further, there are blocks whose diameter is larger than the diameter of the lower extraction port 5, and such huge blocks have to be manually scraped out from the upper manhole 4. Note that the block amount was 9.1% of the total resin amount. Moreover, the resin deposits on the tank inner wall surface 11 near the liquid interface are 1 to 3 cm thick and 40 cm wide.
cm, and was adhered in a ring shape all around the circumference, and although water was applied from the water sprinkling ring 7, it could not be removed. The amount of adhesion was 4.2% of the total amount of resin.
【0009】(実施例2)10%濃度のPVA(ポリビ
ニルアルコール)を80〜90℃まで昇温して完全に溶
解させ、このPVA溶液を反応槽(重合槽)7に仕込み
、酢酸ビニルモノマおよび触媒を滴下するとともに、ジ
ャケット6に蒸気を通して反応槽7を加温し、反応液の
温度を重合が開始される70〜80℃まで上昇させる。
そして、その温度で散水リング7から散水しつつ撹拌翼
2を45rpm の回転速度で回転させて6〜8時間撹
拌し続けてポリ酢酸ビニルをエマルジョン重合させた。
そして、得られた重合体スラリーを下部抜出口5から抜
き出したところ、液界面近傍部およびその上方部の槽内
壁面11および撹拌軸21には付着物がほとんどなく、
ところどころに斑点状に付着物があったのみであった。
また、付着物は上部マンホールから散水すると全て洗い
流すことができた。なお、付着量は0.6 %であった
。(Example 2) PVA (polyvinyl alcohol) with a concentration of 10% was heated to 80 to 90°C to completely dissolve it, and this PVA solution was charged into a reaction tank (polymerization tank) 7, and vinyl acetate monomer and catalyst is added dropwise, and the reaction tank 7 is heated by passing steam through the jacket 6 to raise the temperature of the reaction solution to 70 to 80° C. at which polymerization starts. Then, at that temperature, the stirring blade 2 was rotated at a rotational speed of 45 rpm while water was being sprinkled from the water sprinkling ring 7, and stirring was continued for 6 to 8 hours to emulsion polymerize the polyvinyl acetate. When the obtained polymer slurry was extracted from the lower extraction port 5, there was almost no deposit on the tank inner wall surface 11 and stirring shaft 21 in the vicinity of the liquid interface and above it.
There were only spots of deposits here and there. Additionally, all deposits could be washed away by sprinkling water from the upper manhole. The amount of adhesion was 0.6%.
【0010】(比較例2)散水しなかった以外は実施例
2と同様にして重合体を得た。液界面近傍部の槽内壁面
11には付着物が厚さ1〜3cm、幅30〜40cmで
全周にわたってリング状に付着しており、下部抜出口5
から抜き出したのち、上部マンホール4から散水したが
取れなかった。この付着量は全樹脂量の5.1 %であ
った。(Comparative Example 2) A polymer was obtained in the same manner as in Example 2 except that water was not sprinkled. On the inner wall surface 11 of the tank in the vicinity of the liquid interface, deposits are attached in a ring shape around the entire circumference with a thickness of 1 to 3 cm and a width of 30 to 40 cm.
After pulling it out, water was sprinkled from the upper manhole 4, but it could not be removed. This amount of adhesion was 5.1% of the total amount of resin.
【0011】[0011]
【発明の効果】この発明にかかる反応槽内における樹脂
のブロック化防止方法は、以上のように構成されており
、槽内壁面および撹拌軸への樹脂の付着がなくなり、こ
の付着物の落下による樹脂のブロック化を防止すること
ができる。したがって、製品ロスが減少するとともに、
抜き出し作業も容易にかつ短時間で行えるようになり、
生産性を向上させることができる。また、槽内壁面に付
着物が付着せず、水のみの洗浄で槽内が綺麗になるため
、従来のようにヘラ等で槽壁を洗浄して槽内壁のコーテ
ィング等を傷めたりすることがなくなる。したがって、
槽自体の寿命も延ばすことができる。[Effects of the Invention] The method for preventing resin blocking in a reaction tank according to the present invention is constructed as described above, and prevents resin from adhering to the inner wall surface of the tank and the stirring shaft. Blocking of the resin can be prevented. Therefore, product loss is reduced and
Extraction work can now be done easily and in a short time.
Productivity can be improved. In addition, there is no deposit on the inner wall of the tank, and the inside of the tank can be cleaned by cleaning with water only, so there is no need to clean the tank wall with a spatula or the like as in the past, which could damage the coating on the inner wall of the tank. It disappears. therefore,
The life of the tank itself can also be extended.
【図1】この発明にかかる反応槽内における樹脂のブロ
ック化防止方法を実施するのに用いられる装置の1例を
模式的にあらわす説明図である。FIG. 1 is an explanatory diagram schematically showing an example of an apparatus used to carry out the method for preventing resin blocking in a reaction tank according to the present invention.
1 反応槽 7 散水リング 11 槽内壁面 21 撹拌軸 1 Reaction tank 7. Watering ring 11 Tank inner wall surface 21 Stirring shaft
Claims (1)
望の樹脂を合成する際に反応液中での樹脂のブロック化
を防止する方法であって、反応中、液界面近傍部および
その上方部の反応槽内壁面および撹拌機の撹拌軸に散水
して撹拌等により飛散した反応液中の樹脂の付着を防止
することを特徴とする反応槽内における樹脂のブロック
化防止方法。[Claim 1] A method for preventing resin blocking in a reaction solution when a desired resin is synthesized by reacting raw materials in a reaction tank, the method comprising: A method for preventing resin from forming blocks in a reaction tank, which comprises spraying water on the upper inner wall surface of the reaction tank and the stirring shaft of a stirrer to prevent adhesion of resin in the reaction liquid scattered by stirring or the like.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP1012891A JPH04246423A (en) | 1991-01-30 | 1991-01-30 | Method for preventing resin from blocking in reaction tank |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP1012891A JPH04246423A (en) | 1991-01-30 | 1991-01-30 | Method for preventing resin from blocking in reaction tank |
Publications (1)
Publication Number | Publication Date |
---|---|
JPH04246423A true JPH04246423A (en) | 1992-09-02 |
Family
ID=11741649
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP1012891A Pending JPH04246423A (en) | 1991-01-30 | 1991-01-30 | Method for preventing resin from blocking in reaction tank |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPH04246423A (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2002030103A (en) * | 2000-05-10 | 2002-01-31 | Sekisui Chem Co Ltd | Method for preventing of polymer from adhering |
CN104787507A (en) * | 2015-04-29 | 2015-07-22 | 中煤科工集团武汉设计研究院有限公司 | Large coal slurry storage tank |
-
1991
- 1991-01-30 JP JP1012891A patent/JPH04246423A/en active Pending
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2002030103A (en) * | 2000-05-10 | 2002-01-31 | Sekisui Chem Co Ltd | Method for preventing of polymer from adhering |
CN104787507A (en) * | 2015-04-29 | 2015-07-22 | 中煤科工集团武汉设计研究院有限公司 | Large coal slurry storage tank |
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