KR101776405B1 - Neopentyl glycol manufacturing equipment and preparation method - Google Patents

Neopentyl glycol manufacturing equipment and preparation method Download PDF

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KR101776405B1
KR101776405B1 KR1020150141586A KR20150141586A KR101776405B1 KR 101776405 B1 KR101776405 B1 KR 101776405B1 KR 1020150141586 A KR1020150141586 A KR 1020150141586A KR 20150141586 A KR20150141586 A KR 20150141586A KR 101776405 B1 KR101776405 B1 KR 101776405B1
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neopentyl glycol
hydrogenation reactor
production equipment
supply pipe
catalyst
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KR20160047981A (en
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정다원
엄성식
고동현
김미영
김태윤
최민지
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주식회사 엘지화학
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/132—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of an oxygen containing functional group
    • C07C29/136—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of an oxygen containing functional group of >C=O containing groups, e.g. —COOH
    • C07C29/14—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of an oxygen containing functional group of >C=O containing groups, e.g. —COOH of a —CHO group
    • C07C29/141—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of an oxygen containing functional group of >C=O containing groups, e.g. —COOH of a —CHO group with hydrogen or hydrogen-containing gases
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C31/00—Saturated compounds having hydroxy or O-metal groups bound to acyclic carbon atoms
    • C07C31/18—Polyhydroxylic acyclic alcohols
    • C07C31/20—Dihydroxylic alcohols

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  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The present disclosure relates to an apparatus and a method for producing neopentylglycol, and it is an object of the present invention to provide a process for producing neopentylglycol by removing metal particles that can be separated from the fixed bed of a hydrogenation reactor during the reaction, thereby suppressing side reactions in subsequent processes, It is possible to make continuous flow only by a small amount of liquid drawn from the recirculation supply pipe without any extra energy or large modification of the existing piping, and thus a very economical production apparatus and a catalyst-derived metal particle free of the use of neopentyl glycol There is an effect of providing a manufacturing method.

Description

[0001] NEOPENTYL GLYCOL MANUFACTURING EQUIPMENT AND PREPARATION METHOD [0002]

The present disclosure relates to an apparatus and a method for producing neopentylglycol, and it is an object of the present invention to provide a process for producing neopentylglycol by removing metal particles that can be separated from the fixed bed of a hydrogenation reactor during the reaction, thereby suppressing side reactions in subsequent processes, It is possible to make continuous flow only by a small amount of liquid drawn from the recirculation supply pipe without any extra energy or large modification of the existing piping, and thus a very economical production apparatus and a catalyst-derived metal particle free of the use of neopentyl glycol And a manufacturing method thereof.

Neopentyl glycol (NPG) is a white crystalline material with a melting point of 129.13 ℃. It is used as an important intermediate for various synthetic resins. It is also used as a raw material for various plastic powder coatings, synthetic lubricants, plasticizers, surfactants, It is widely used.

Generally, NPG is produced by the reaction of isobutyraldehyde and formaldehyde by aldol condensation to form hydroxypivaldehyde (HPA), and then this HPA is reacted with hydrogen under a catalyst as shown in the following reaction formula (1).

[Reaction Scheme 1]

Figure 112015097659297-pat00001

Conventional devices for making NPG include feed vessels; A raw material feed pipe for feeding hydroxypivalic aldehyde from the feed roll to the hydrogenation reactor; A hydrogen supply pipe for supplying hydrogen to the hydrogenation reactor; A hydrogenation reactor including a hydrogenation catalyst therein; And a discharge pipe for discharging the neopentyl glycol product produced from the hydrogenation reactor, wherein the hydroxypivalicdehyde is fed from the feed bead to the hydrogenation reactor through a feed pipe, and hydrogen is fed through the feed pipe to the hydrogenation reactor And reacted under a hydrogenation catalyst in the hydrogenation reactor to produce neopentyl glycol. The resulting neopentyl glycol is discharged through a discharge pipe, and a portion of the produced neopentyl glycol is further introduced into the hydrogenation reactor.

Here, when the catalyst-derived metal particles are separated from the fixed bed in the hydrogenation reactor and contained in the neopentyl glycol product discharged through the exhaust pipe in an amount exceeding a certain amount in ppm, the decomposition of neopentyl glycol or generation of heavies There is a problem of performing the same side reaction.

KR Patent Publication No. 2006-0103504 (published on October 2, 2006)

In order to solve the problems of the prior art as described above, the present invention eliminates the metal particles that can be separated from the fixed layer of the hydrogenation reactor during the reaction, thereby suppressing the side reaction in the subsequent process, The present invention provides a highly economical production apparatus and a method for producing free metal particle free neopentyl glycol using the same, since continuous flow can be made only by a small amount of liquid drawn from the recirculation supply pipe without entering or without large modification of the existing piping .

In order to achieve the above object, the present invention relates to a feed vessel in which a hydroxypivalate solution is stored; A raw material feed pipe for feeding the hydroxypivalic aldehyde solution from the feed roll to the hydrogenation reactor; A hydrogen supply pipe for supplying hydrogen to the hydrogenation reactor; A hydrogenation reactor including a hydrogenation catalyst therein; A discharge pipe for discharging the neopentyl glycol product produced from the hydrogenation reactor; And a recycle line for recycling the neopentyl glycol product from the discharge line to the hydrogenation reactor,

And a liquid stream supply line connected to the recycle line,

And a strainer and a filter are provided on the liquid stream supply pipe.

The present disclosure also provides a process for preparing free neopentyl glycol from a catalyst-derived metal particle using the above-described production apparatus.

As described above, according to the present invention, by removing metal particles that can be separated from the fixed bed of the hydrogenation reactor during the reaction, the side reaction is suppressed in the subsequent process, and continuous flow is generated without any additional power, It is possible to make continuous flow only with a small amount of liquid drawn out from the recirculation feed pipe without a large modification of the piping, thereby providing a very economical manufacturing apparatus and a method for producing free metal neopentyl glycol using the catalyst.

BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a process diagram schematically showing an apparatus for producing neopentyl glycol according to the present invention. FIG.

Hereinafter, the present invention will be described in more detail on the basis of a schematic process drawing of the neopentyl glycol production process of FIG. 1.

The apparatus for producing neopentyl glycol according to the present invention comprises a feed vessel 1 in which a solution of hydroxypivalic aldehyde is stored; A raw material feed pipe 2 for feeding the hydroxypivalate solution from the feed roll 1 to the hydrogenation reactor 7; A hydrogen supply pipe (5) for supplying hydrogen (4) to the hydrogenation reactor (7); A hydrogenation reactor (7) containing a hydrogenation catalyst therein; A discharge pipe (8) for discharging the neopentyl glycol product produced from the hydrogenation reactor (7); And a recycle piping (11) for recycling the neopentyl glycol product from the discharge pipe (8) to the hydrogenation reactor (7), wherein the liquid stream connected to the recycle line (11) a liquid stream supply pipe 12 and a strainer 13 and a filter 14 on the liquid stream supply pipe 12.

The apparatus for producing neopentyl glycol according to the present invention can be, for example, a catalyst-derived metal particle free neopentyl glycol production apparatus.

The term "free of catalyst-derived metal particles " as used herein means that, when the metal particles are separated from the fixed bed catalyst in the hydrogenation reactor 7, they are efficiently filtered Quot;

For reference, in the presence of the catalyst-derived metal particles in the subsequent process, neopentyl glycol may be thermally decomposed by metal particles such as copper under high temperature in the distillation process or may produce various heavies components as a side reaction result.

The raw material supply pipe is provided with a pre-heater 3, and preferably a solution of the hydroxypivalic aldehyde supplied from the feedblend 1 is maintained at 25 to 160 캜, or 50 to 80 캜 To the hydrogenation reactor (7). In this case, there is an effect of minimizing the production of by-products while preventing crystallization of hydroxypivalic aldehyde.

The hydroxypivalic aldehyde solution may include, for example, 10 to 50% by weight of hydroxypivalaldehyde, 20 to 80% by weight of neopentyl glycol and 10 to 30% by weight of water. In this case, The heating can be minimized and the production of by-products can be suppressed.

In another example, the hydroxypivalaldehyde solution may comprise from 10 to 30% by weight of hydroxypivalate, from 45 to 70% by weight of neopentyl glycol and from 0 to 20% by weight of water, The reaction heat can be minimized and the production of by-products can be suppressed.

The hydroxypivalic aldehyde solution can be prepared in advance in a feed vessel 1, for example. In this case, the entire manufacturing process can be operated stably and the operation is easy.

In the apparatus for producing neopentyl glycol, the hydrogen supply pipe 5 is connected to the raw material supply pipe 2, and in this case, the hydrogenation reaction yield and the hydroxypivalate conversion are excellent.

The apparatus for producing neopentyl glycol includes a recycling pipe 11 for recycling some neopentyl glycol product from the discharge pipe 8 to the hydrogenation reactor 7, thereby facilitating heat removal, have.

The recycling pipe 11 may be connected to the raw material supply pipe 2 for example.

The neopentyl glycol production apparatus may further include a neopentyl glycol recovery pipe (not shown) for supplying some neopentyl glycol product from the discharge pipe 8 to the feed chain 1, The aldehyde is easily liquefied, the process is economical and the process efficiency is good.

A static mixer (not shown) may be provided between the portion where the recycle pipe 11 and the raw material supply pipe 2 are connected and the inlet of the hydrogenation reactor 7. In this case, And stirring effect, and maximizing the effect of dispersing into the catalyst layer when introduced into the reactor, thereby increasing the yield of neopentyl glycol.

The liquid stream may be, for example, neopentylglycol (NPG) or various materials contained in the raw material, and may or may not contain hydroxypivalic aldehyde as a reactant.

The liquid stream supply pipe 12 may be connected before the point where the recycle pipe 11 is first bent to supply the liquid stream.

The liquid stream supply pipe 12 may be branched from the recirculation supply pipe 11, and in this case, it is possible to make a continuous flow with only a small amount of liquid drawn out from the recycle supply pipe 11 without large modification of the existing pipe There is an economical effect.

The liquid stream supply pipe 12 may further include a valve 13 at a connection portion with the recycle pipe 11, for example, in which case the flow rate of the liquid stream can be adjusted as needed.

The liquid stream may be supplied to the recycling line 11 continuously or intermittently, for example.

For example, the strainer 14 may have an average pore size of 0.01-1 mm or 0.1-1 mm, and the outer mesh may have a mesh structure of 10-300 mesh or 10-200 mesh. It is preferable to use a screen type filter having the above-described structure, because the filtration process can be efficiently performed without delaying the discharge speed or the like.

The filter is not limited to this. For example, the filter may have an average pore size of 2.0 mu m, a filtration area of 2000 cm < 2 > An average pore size of 1.0 mu m, a filtration area of 2000 cm < 2 > And three filters having an average pore size of 0.2 mu m and a filtration area of 1800 cm < 2 > are connected in series in the order of a large filter pore size, because the filtration process can be efficiently performed without delaying the discharge speed and the like.

It is preferable that the strainer and the filter are sequentially provided from the viewpoint of filtration efficiency.

As a specific example, the neopentyl glycol product discharged into the liquid stream feed pipe 12 is subjected to continuous filtration (50 ° C under hydrogen pressurization of 3 kgf / cm 2) while passing through the strainer 14 and the filter 15, The ratio of the filtration rate after one hour to the filtration rate after 10 hours can be maintained in the range of 0.85 to 1.00, or 0.90 to 1.00.

It is preferable that the neopentyl glycol product discharged into the liquid stream supply pipe 12 has a solid concentration of 1.0 wt% or less.

A distributor 6 may be installed at the top of the hydrogenation reactor 7, and in this case, the reaction yield, the hydroxypivalate conversion, and the neopentyl glycol selectivity are excellent.

The exhaust pipe 8 may be provided with a pump 9 and a heat exchanger 10. In this case, the heat generated in the hydrogenation reaction is easily controlled.

The pump 9 and the heat exchanger 10 can be located before the recycling pipe 11, for example, and have high process efficiency and little by-product production.

The pump 9 is located, for example, before the heat exchanger 10, and in this case, the process efficiency is high and the clogging phenomenon of the pipe is reduced.

The discharge pipe 8 may be, for example, a down slope discharge pipe leading to the heat exchanger 10 without a corner and downslope. In this case, clogging of the pipeline is prevented to prevent time and equipment trouble The piping is blocked and the operation is not interrupted. Therefore, the production amount is increased. Also, when the reaction is stopped after a certain period of reaction, the line cleaning operation is not necessary and continuous flow is made without any additional power Separate energy is unnecessary.

The liquid stream supply pipe 12 having passed through the strainer 9 and the filter 15 can be connected to the neopentyl glycol distillation device 16 in this case and the metal particles of the catalyst are free It is possible to prevent neopentyl glycol from decomposing under high temperature of distillation or from generating heavy components by other side reaction.

The hydrogenation reactor 7 is, for example, a fixed bed reactor. In this case, the hydrogenation reactor 7 is easy to work, produces energy for neopentyl glycol production, has a simple purification facility, and has a low purification cost.

The fixed bed reactor may be, for example, a Ni-based catalyst or a Cu-based catalyst, and in the case of a Cu-based catalyst, the performance of the catalyst is excellent and the lifetime is long.

The copper-based catalyst is, for example, a CuO / BaO catalyst. In this case, the performance of the catalyst is excellent and the lifetime is long.

The CuO / BaO catalyst includes, for example, CuO in an amount of 10 to 50% by weight and BaO

And 50 to 90% by weight, and preferably a CuO / BaO catalyst containing 30 to 50% by weight of CuO and 50 to 70% by weight of BaO, more preferably a CuO / BaO catalyst containing 35 to 35% By weight to 45% by weight and BaO in an amount of 55 to 65% by weight. Within this range, the catalyst is excellent in performance and has a long service life.

As another example, the CuO / BaO catalyst is a CuO / BaO catalyst containing 60 to 99 wt% of CuO and 1 to 40 wt% of BaO, preferably containing 80 to 95 wt% of CuO A CuO / BaO catalyst containing 5 to 20% by weight of BaO, more preferably a CuO / BaO catalyst containing 85 to 90% by weight of CuO and 10 to 15% by weight of BaO, The performance of the catalyst is excellent and the lifetime is long.

The CuO / BaO catalyst can measure metal and metal oxide contents by ICP analysis as an example.

The copper-based catalyst may include, for example, a silicon oxide or an aluminum oxide support. In this case, the performance and physical properties of the catalyst are good and the activity of the catalyst is maintained for a long time.

The copper-based catalyst may preferably be a CuO / BaO / SiO catalyst.

(CuO) x (BaO) y (SiO) z wherein x, y and z are weight percent and x: y: z = 10 to 50: 0 to 20:40 to 90 , 10 to 50: 1 to 20:40 to 89 or 29 to 50: 1 to 10:40 to 70). The sum of x and y is preferably 20 to 50 (wt%), or 30 to 50 (wt%) based on the total of x, y and z (100 wt% Is excellent and has a long lifetime effect.

The feed ballast 1 may be connected to an aldol condensation reaction apparatus (not shown). In this case, the feed liquid 1 can be directly supplied with the hydroxypivalic aldehyde produced from the agglomeration reaction apparatus (not shown) This has an excellent effect.

The process for producing neopentyl glycol according to the present invention comprises the preparation of free neopentyl glycol from a catalyst-derived metal particle using the above-described production apparatus.

For example, the neopentylglycol product discharged from the production apparatus to the reaction liquid stream supply pipe is subjected to continuous filtration (50 ° C under hydrogen pressurization of 3 kgf / cm 2) while passing through the strainer 14 and the filter 15, The ratio between the filtration rate after 1 hour and the filtration rate after 10 hours from 0.85 to 1.00, or 0.90 to 1.00 can be maintained.

That is, using a device including a liquid stream feed pipe 12 connected to the recirculation pipe 11 according to the present invention and having a strainer 14 and a filter 15 on the liquid stream feed pipe 12 It is possible to efficiently filter the metal particles which can be separated from the fixed layer in the hydrogenation reactor 7 and to produce economical neopentyl glycol because no separate energy power is required and the obtained catalyst- free) neopentyl glycol can be purified through a purification process such as distillation.

Hereinafter, preferred embodiments are shown to facilitate understanding of the present invention, but the present invention is not limited to the following examples.

Example  One

As shown in FIG. 1, a feed ball 1, a preheater 3, a hydrogen source 4, a distributor 6, a hydrogenation reactor 4, Neopentyl glycol was prepared using a production apparatus comprising a pump 7, a pump 9, a heat exchanger 10, a discharge valve 13, a strainer 14, and a filter 15.

10 to 50 wt% of hydroxypivalic aldehyde, 20 to 80 wt% of neopentyl glycol and 10 to 30 wt% of water were fed to a 5 L capacity feed barrel (1) While being transferred to the hydrogenation reactor 7 at a flow rate of 3 g / min through the raw material supply pipe 2. At the same time, the hydrogen (4) is introduced into the raw material supply pipe (2) through the hydrogen supply pipe (5) and mixed with the hydroxypivalic aldehyde solution. Part of the neopentyl glycol product produced after the hydrogenation reaction is discharged through the discharge pipe And recycled through the recycle piping 11 via the pump 9 and the heat exchanger 10. At this time, the catalyst fixed to the hydrogenation reactor 7 was CuO / BaO / SiO (CuO: BaO: SiO weight ratio = 40: 5: 55) catalyst, and the reaction temperature and the reaction pressure were 130 ° C. and 35 bar, respectively.

After 24 hours of continuous operation, the neopentylglycol product produced from the hydrogenation reactor 7 was discharged through the discharge valve 13 to transfer some recycle from the recycle piping 11 to the liquid stream supply line 12, A screen type strainer 14 having an average pore diameter of 0.1-1.0 mm and a mesh type mesh structure of 10-300 mesh as an external network and a strainer 14 having an average pore size of 2.0 탆 , Filtration area 2000 cm < 2 & gt ;; An average pore size of 1.0 mu m, a filtration area of 2000 cm < 2 > And a filter 15 in which three filters having an average pore size of 0.2 mu m and a filtration area of 1800 cm < 2 > were connected in series in the order of a large filter pore, were sequentially passed through, and the recycled material had a solid concentration of less than 1.0 wt%.

The neopentylglycol product discharged into the liquid stream supply pipe 12 is passed through the strainer 14 and the filter 15 for continuous filtration (under the conditions of 50 ° C and hydrogen pressurization of 3 kgf / cm 2 ) And the ratio of the filtration rate after the filtration to the filtration rate after 10 hours was 0.85 to 1.00.

The composition of the obtained neopentyl glycol product was measured using gas chromatography (HP-1, Agilent, measuring conditions: 70 ° C / 3min-10 ° C / min-280 ° C / 35min ° C) (NPG) of 67.1%, and heavies containing hydroxypivalic acid neopentyl glycol ester (HPNE) (5.7%).

Example  2

In the first embodiment, the stripliner 14 has an average pore diameter 0.1 to 5 mm, and the external network is a screen having a mesh structure of 10 to 200 meshes The same experiment as in Example 1 was repeated except for the screen type.

As a result, the recycled material had a solid concentration of 1.3 wt%, and the neopentyl glycol product discharged to the liquid stream feed pipe 12 was fed to the strainer 14 During continuous filtration (50 ° C under hydrogen pressurization of 3 kgf / cm 2) while passing through the filter 15, filtration When the ratio of the filtration rate after 1 hour from the start and the filtration rate after 10 hours is 0.9 To 1.00, and the composition of the obtained neopentyl glycol product was changed to gas As a result of measurement using chromatography (HP-1, Agilent, measuring conditions: 70 ° C / 3min-10 ° C / min-280 ° C / 35min ° C), 66.5% of NPG and 6.0% of heavies containing HPNE there was.

Example  3

In the first embodiment, the filter 15 has an average pore size of 0.01-1.0 mm in the perforated network constituting the water receiving portion, and the external network is the screen having the mesh structure of 10-500 mesh The same experiment as in Example 1 was repeated except for the screen type.

As a result, the recycled material had a solids concentration of less than 0.5% by weight, The neopentyl glycol product discharged into the stream supply pipe 12 flows through the strainer 14 During continuous filtration (50 ° C under a nitrogen pressure of 3.0 kgf / cm 2) while passing through the filter 15, filtration The ratio of the filtration rate after 1 hour from the start and the filtration rate after 10 hours was 0.3 To 0.85, and the composition of the obtained neopentyl glycol product was changed to gas As a result of measurement using chromatography (HP-1, Agilent Co., measurement conditions: 70 ° C / 3min-10 ° C / min-280 ° C / 35min ° C), 67.9% of NPG and 675.1% of heavies containing HPNE there was.

Comparative Example  One

In the above-mentioned Embodiment 1, the case where neither the strainer 14 nor the filter 15 is passed The same experiment as in Example 1 was repeated.

As a result, the recycled material had a solid concentration of 8 wt%, and the liquid stream The composition of the neopentyl glycol product discharged into the feed pipe 12 is referred to as gas The measurement was carried out using chromatography (HP-1, Agilent, measuring conditions: 70 ° C / 3min-10 ° C / min-280 ° C / 35min ° C). As a result, NPG 67.0%, heavies containing HPNE 5.9%.

Comparative Example  2

In the first embodiment, after passing through the strainer 14 and then passing the filter 15 The same experiment as in Example 1 was repeated.

As a result, the recycled material had a solids concentration of 5.6 wt% and the gas stream The neopentyl glycol product discharged into the feed pipe 12 flows through the strainer 14 During continuous filtration (50 ° C under hydrogen pressurization of 3.0 kgf / cm 2) while passing through the filter 15, filtration When the ratio of the filtration rate after 1 hour from the start and the filtration rate after 10 hours is 0.9 To 1.0, and the composition of the obtained neopentyl glycol product was changed to gas The measurement was conducted using chromatography (HP-1, Agilent, measuring conditions: 70 ° C / 3min-10 ° C / min-280 ° C / 35min ° C). As a result, NPG was found to be 65.9% heavies were 5.8%.

Comparative Example  3

In the first embodiment, the filter 15 is passed without passing the strainer 14, The same experiment as in Example 1 was repeated.

As a result, the recycle had a solids concentration of 1.7% by weight and the gas stream The neopentyl glycol product discharged into the feed pipe 12 flows through the strainer 14 During the continuous filtration (50 DEG C under hydrogen pressurization of 3.0 kgf / cm < 2 >) while passing through the filter 15, filtration The ratio of the filtration rate after 1 hour from the start and the filtration rate after 10 hours 0.85 to 1.0, and the composition of the obtained neopentyl glycol product was changed to gas As a result of measurement using chromatography (HP-1, Agilent, measuring conditions: 70 ° C / 3min-10 ° C / min 280 ° C / 35min ° C), 67.3% of NPG and 5.4% of heavies containing HPNE .

Manufacturing example  1 to 2

The neopentyl glycol product obtained in Example 1 and the product obtained in Comparative Example 1 The neopentyl glycol product is fed into distillation columns of 3 to 15 stages respectively, The distillation process was carried out under the temperature condition.

As a result of GC analysis of the resulting final product, it was confirmed that the neopentyl glycol obtained in Example 1 When the product was used, the degradation rate of NPG and the yield of heavies were less than 1%, so that no decomposition of neopentyl glycol or generation of other heavy components could be observed.

On the other hand, when using the neopentyl glycol product obtained in Comparative Example 1, neopentyl glycol was obtained by providing 7.9% of NPG and 7.8% of heavies, 0.9% decomposition, and the heavy component including PNE increased by 1.9%.

Thus, Examples 1 to 3 according to the present invention can efficiently filter metal particles that can be separated from the fixed bed in the hydrogenation reactor 7 to a degree sufficient to suppress side reactions in the subsequent processes as compared with Comparative Examples 1 to 3, Neopentyl glycol can be economically produced because no separate energy power is required.

1: feed vessel
4: Hydrogen source
7: Hydrogenation reactor
12: Liquid stream supply piping
14: Strainer
15: Filter

Claims (15)

A feed vessel in which a solution of hydroxypivalic aldehyde is stored; A raw material feed pipe for feeding the hydroxypivalic aldehyde solution from the feed roll to the hydrogenation reactor; A hydrogen supply pipe for supplying hydrogen to the hydrogenation reactor; A hydrogenation reactor including a hydrogenation catalyst therein; A discharge pipe for discharging the neopentyl glycol product produced from the hydrogenation reactor; And a recycle line for recycling the neopentyl glycol product from the discharge line to the hydrogenation reactor,
And a liquid stream supply line connected to the recycle line,
Characterized in that a strainer and a filter are provided on the liquid stream supply pipe
Neopentyl glycol production equipment. The method according to claim 1,
Characterized in that the raw material supply pipe is provided with a pre-heater
Neopentyl glycol production equipment. The method according to claim 1,
And the hydrogen supply pipe is connected to the raw material supply pipe
Neopentyl glycol production equipment. The method according to claim 1,
Characterized in that the recycling line is connected to a raw material supply line
A device for producing neopentyl glycol. The method according to claim 1,
Wherein the neopentyl glycol production apparatus further comprises a neopentyl glycol recovery line for feeding some neopentyl glycol product from the discharge line to the feed bead
Neopentyl glycol production equipment. The method according to claim 1,
Characterized in that the liquid stream comprises at least one of neopentyl glycol product, the material contained in the raw material, and hydroxypivalaldehyde
Neopentyl glycol production equipment. The method according to claim 1,
Wherein the strainer is a screen type having an average pore diameter of 0.01-1 mm and an external network having a mesh structure of 10-100 mesh,
Neopentyl glycol production equipment. The method according to claim 1,
The filter had an average pore size of 2.0 mu m, a filtration area of 2000 cm < 2 > An average pore size of 1.0 mu m, a filtration area of 2000 cm < 2 > And three filters having an average pore diameter of 0.2 mu m and a filtration area of 1800 cm < 2 > are connected in series in the order of a large filter pore diameter
Neopentyl glycol production equipment. The method according to claim 1,
At the top of the hydrogenation reactor, a distributor is installed
Characterized by
Neopentyl glycol production equipment. The method according to claim 1,
Characterized in that the recycling line is provided with a pump
Neopentyl glycol production equipment. The method according to claim 1,
Characterized in that the recycling line is provided with a heat exchanger
Neopentyl glycol production equipment. The method according to claim 1,
Characterized in that the hydrogenation reactor is a fixed bed reactor
Neopentyl glycol production equipment. A process for the production of free neopentyl glycol from a catalyst-derived metal particle using the production apparatus of any one of claims 1 to 12,
Method for preparing neopentyl glycol. 14. The method of claim 13,
During the production, the neopentylglycol product discharged into the reaction liquid stream supply pipe of the production apparatus was subjected to continuous filtration (50 ° C under hydrogen pressurization of 3 kgf / cm 2 ) while passing through a strainer and filter, filtration after 1 hour from the start of filtration Characterized in that the ratio of the velocity to the filtration rate after 10 hours is maintained between 0.85 and 1.00
Method for preparing neopentyl glycol. 14. The method of claim 13,
Wherein the catalyst-derived metal particle free neopentyl glycol further comprises a purification process
Method for preparing neopentyl glycol.
KR1020150141586A 2014-10-23 2015-10-08 Neopentyl glycol manufacturing equipment and preparation method KR101776405B1 (en)

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