JPS6049011A - Device for vapor-phase polymerization of vinyl chloride - Google Patents

Abstract

PURPOSE:The titled device providing a porous polymer having high bulk specific gravity, provided with a spray nozzle for a vinyl chloride monomer, a spray nozzle for seed polymer slurry, a line for recovering the monomer, an anchor-shaped blade, a pipe for extracting a product, having a specific diameter, and jackets. CONSTITUTION:Polymerization is carried out to give a high-quality polymer by a polymerizer wherein the whole reactor 1 for homopolymerization or copolymerization of vinyl monomer is covered with the jackets 2-4 divided at least into two parts at the top and bottom, the spray nozzle 9 for feeding the vinyl chloride monomer to the reactor 1, the spray nozzle 10 for seed polymer slurry for feeding the seed polymer, the line 16 for recovering the gas of the vinyl chloride monomer, the anchor-shaped blade 5 having length 1/4-1/2 that of the barrel of the reactor, and the pipe 7 for extracting prepared polymer from the bottom to the top in the reactor 1, having >=25Angstrom diameter, are set.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention involves continuous polymerization using a stirring method in gas phase polymerization of bulk vinyl monomers (abbreviated as VCM) or a comonomer that can be copolymerized mainly with agglomerated vinyl monomers (abbreviated as VCM). The present invention relates to a reaction apparatus suitable for carrying out the process.

Regarding the gas phase polymerization of VOM, Japanese Patent Publication No. 48-1466
6, Special Publication No. 52-44918. U.S. Patent 5,578.6
46, etc., but the quality of the product obtained was insufficient.

The inventors, as a result of intensive research, found that the conventional gas phase polymerization method is possible!
It has been found that it is possible to obtain a product that is sufficiently comparable to a legal product of 1 turbidity and 1f or a two-stage mass polymerized product using a semi-continuous or continuous summer method. That is, ① The properties of the polymer, which is the starting point of all aspects of gas phase polymerization, have a dominant influence on the properties of the gas phase polymerized product.

11, when carrying out polymerization with a polymerization rate of 14 to 25φ by bulk prepolymerization, the C1 quadrature distribution should be sharpened (and the internal structure of the particles should be changed, and the particles should be Adding a special additive to prevent the internal bulge from occurring, and coating the particle surface with a special additive HA 11 at the end of polymerization; It prevents percolation and internal weight, and also prevents agglomeration between particles.Furthermore, when recovering unreacted VGM and making it into a powder polymer, sufficient stirring shear and heat must be applied. The aim is to reduce the unevenness of the particle surface and create a unique polymer with relatively good bulk density and good porosity.

■ Gas-phase polymerization Gas-phase polymerization can be carried out at Pr (saturated vapor pressure of VCM at combined pressure PO/polymerization temperature P8) less than 1 or more than a5, but if Pr is high, the reactivity will be low and the bulk ratio will be significant. The particle size becomes Itoyab.

The incidence of coarse particles is also reduced. In addition, the hue + PA during product processing
Stability is also improved, but the fishy eye characteristic (hereinafter referred to as FE)
Characteristics and abbreviations) deteriorate.

Therefore, in order to keep the lj'11 characteristics at a good level and the other physical properties at a practical level, we
It is necessary to carry out the gas phase polymerization at a concentration of 5 to 0.85, preferably 0.70 to 0.85.

C4: If the multiplication ratio exceeds 5 to 6 times, the properties of the product in the next process will deteriorate. , it is necessary to always maintain the growth ratio within a range of 65 to 55 times.

■IIL synthesis slurry - As a means of supplying atomized e-polymer, it is most rational from a process standpoint to supply a slurry with a polymerization rate of 14 to 25 by bulk prepolymerization using 11Q thread. There are some problems. The biggest problem among these is that aggregated coarse particles are likely to occur.

Since the polymer slurry ei has a smaller particle diameter and is softer than the powdered extracted polymer, it is thought that it acts as a binder by acting as a binder on the gas phase polymerized powder, and is likely to cause agglomerated coarse particles.

There are several measures to prevent the generation of agglomerated coarse particles, but the main ones are (a) Add an additive effective in preventing hood collection to the stopper slurry in advance.

(-14 Stir thoroughly and uniformly to prevent M nests.

(c) When Pr is V, the particles are almost in a wet state and a sufficient amount of anti-lb heat is used, so agglomeration is less likely to occur.

Therefore, as a stirred gas phase polymerization apparatus, the key points that should be avoided are:
As a plus, 1) The whole can be stirred homogeneously.If the size of the can is large, stir it from the bottom with an anchor-shaped blade as shown in Figure 1. The rotational speed is preferably 40 to 80 rpm with low speed stirring of 100 rpm or less. Also, it is desirable that the shaft be oiled so that it has a hollow hole so that the temperature detection end can be inserted therein. The length of the anchor blade must be at least 1/4 of the straight body length in order to stir sufficiently up to the top.
There is no need to make it too long, but to prevent the ingredients from wobbling, make it 1/2.
It is best to do the following: - Stop.If the 44 stirring in the upper part of the medium heat becomes uneven, either lower the 1lIII from the upper part and attach an aileron, or (rl, extend the lower shaft and add an auxiliary blade. Attach wings.

2) The jacket covers the entire reaction tank and covers the soil.

Divide it into two or more parts downward. The upper part of the jacket is designed to prevent scaling from rain, so the applied temperature is maintained slightly higher to prevent the generation of liquefied VCM.

The Juto jacket always has a powder layer in contact with the edges.
Even if IN conversion V Ohi occurs due to C1 cooling, it is moot +>
'As the body wipes, scaling occurs.

1. Furthermore, there is a small ability to cool and remove heat.

6b) It is preferable to provide a split C intermediate fXIs jacket. At the start of 11i, this was used for heating to prevent scale generation and rain, as was the case with part 1-E, and the powder layer was sufficiently -F.
3) It is possible to extract the product from the bottom of the can, but if the ten-valve seal fails, it is difficult to maintain the reaction pressure, so it is difficult to remove the product from the bottom of the can. ;1? is used for emergency purposes, and is used for regular driving.
From the top, use a size 25A1 test tube to remove a pipe of a size that matches the amount you need to extract.4. To explain this in Figure 1, open the automatic valve (preferably a ball valve) A, send water to the control pipe (+W not shown) between A and B, close A, and then automatically Open valve B and send to the low pressure system charge tank. The product powder can be easily pumped because of the stirring bit.

Payout/1 to 9 of C for the purpose of preventing internal scaling
It is effective to extract with a small automatic valve and flush the inside of the extraction pipe with nitrogen at market pressure once every 10 to 10 times.

4) h order of the spray nozzle a V C+, (and liquid delivery u of heavy-containing sour free: V according to kC
C) Installation of InnoX'le and slurry nozzle 1'7. −
'J-ru. .

V
．． A swirling flow of more than 5 residences φ! (Lisbrae nozzle is best, 2
B1. It is desirable to install 1ffi of J or more. 3. If the slurry nozzle is too large, it will stagnate, and if it is too small, it will tend to clog. Good nozzle, installation of 2 or more
is desirable.

5) Cyclone polymerization heat in the recovery gas line is removed using VOM spray or the latent heat of vaporization of unreacted VCM in the slurry. In order to keep the reaction pressure constant, excess gas is discharged from the control valve to the recovery line via a pressure regulator (17i'l), but since a small amount of fine polymer is entrained, a cyclone must be set up. .

For continuous ljc polymerization, there is a possibility of clogging due to scaling due to long-term use, so it is desirable to double the casfin up to Zykron so that it can be switched and cleaned.

6) Adjustment method Slurry feed 1 is kept constant, cooling water temperature and water flow in the lower jacket are constant, and one of the items is adjusted using VClAI.
(The method of core-1-rolling the supply pump flow iA' is most difficult.

41v 1 side quick 1st situation Akira 7A31 figure is one implementation of non-invention) i! ! 4 types of gas phase)E
l=I, which indicates the pin length 11 of the combining device d.

1: Can body 2: Upper jacket 3: Middle jacket 4: Lower jacket 5: Anchor type 1N stirring blade agitator 6: Discharge valve 7: Product extraction pipe 8: Strip type stirring blade Stirring type 9: Spray for single container body Nozzle 10: Spray nozzle 11 for yuzu polymer slurry Recovery gas cyclone 12; Vinyl chloride monomer supply line 15: Seed polymer slurry supply line 14.15: Product polymer discharge line 16; Vinyl chloride monomer recovery Special fraud applicant: Toyo Soda Shigei Co., Ltd.

Claims (1)

[Claims] (n 1 = vinyl chloride single 111 polymer or co-i8', blowing bond nozzle for cyclized vinyl monomer, single shell spray nozzle for German polymer slurry, vinyl chloride 4i polymer slurry) In the gas-phase polymerization apparatus a of y!I, which includes a gas recovery line, agitation (vertical, vertical pipe, product discharge pipe, and jacket), (a) the blade length is 1/4 to 1/2 of the length of the reactor body. Anchor tension], No5 Stirring 0]) Pull out the combined product from the bottom of the reaction can to -F, and remove the V product with a diameter of 25A or more.(C) The entire reaction can A gas phase polymerization apparatus m characterized by having a jacket divided into at least two parts above and below.(21Sr°6 type 4 stirring ports θ') (3) A rectangular type (a device equipped with a birthing agitator as an auxiliary tool)
Claims No. (1)' or (2)
, (4) The nozzle for atomizing polyvinyl chloride (monocarbon) is a human []
Inside r = 1.5 rtr+ or more, inside exit (% 2.0
,,・1 or more - Must be C, and glaze polymer sla')
Exit 2. Or, 1. (2) Service or (equipment described in Section 411) (5) There are two systems of recovery fans for vinyl chloride monomer gas, and each The apparatus according to any one of claims (1) to (.■), which is equipped with pressure equipment.