KR970004909B1 - Rotary vacuum filter to recover crystals from slurry - Google Patents
Rotary vacuum filter to recover crystals from slurry Download PDFInfo
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- KR970004909B1 KR970004909B1 KR1019930032159A KR930032159A KR970004909B1 KR 970004909 B1 KR970004909 B1 KR 970004909B1 KR 1019930032159 A KR1019930032159 A KR 1019930032159A KR 930032159 A KR930032159 A KR 930032159A KR 970004909 B1 KR970004909 B1 KR 970004909B1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D33/00—Filters with filtering elements which move during the filtering operation
- B01D33/06—Filters with filtering elements which move during the filtering operation with rotary cylindrical filtering surfaces, e.g. hollow drums
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D33/00—Filters with filtering elements which move during the filtering operation
- B01D33/44—Regenerating the filter material in the filter
- B01D33/46—Regenerating the filter material in the filter by scrapers, brushes nozzles or the like acting on the cake-side of the filtering element
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C63/00—Compounds having carboxyl groups bound to a carbon atoms of six-membered aromatic rings
- C07C63/14—Monocyclic dicarboxylic acids
- C07C63/15—Monocyclic dicarboxylic acids all carboxyl groups bound to carbon atoms of the six-membered aromatic ring
- C07C63/26—1,4 - Benzenedicarboxylic acid
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
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- Cleaning By Liquid Or Steam (AREA)
Abstract
내용 없음.No content.
Description
제1도는 본 발명에 따르는 회전진공필터가 장치된 테레프탈산 제조장치의 개략도.1 is a schematic view of a terephthalic acid production apparatus equipped with a rotary vacuum filter according to the present invention.
제2도는 제1도에 도시된 회전진공필터의 확대 단면도.2 is an enlarged cross-sectional view of the rotary vacuum filter shown in FIG.
* 도면의 주요부분에 대한 부호의 설명* Explanation of symbols for main parts of the drawings
1 : 회전진공필터 2 : 케이싱1: rotary vacuum filter 2: casing
3 : 횡원통형 여과매체 4 : 슬러리섬프3: lateral cylindrical filter medium 4: slurry sump
5 : 여과영역 5 : 여과액5: filtration area 5: filtrate
7 : 내부가스 8 : 흡인부7: internal gas 8: suction
9 : 케이스 10 : 세정액분사수단9: case 10: cleaning liquid spraying means
11 : 세정영역 12 : 탈액영역11: washing zone 12: dewatering zone
13 : 블로우부(blow horn) 13a : 가스밀폐부13: blow horn 13a: gas seal
14 : 케이크 제거영역 15 : 가스공급부14: cake removal area 15: gas supply unit
16 : 데드 존(dead zone) 17 : 가성소다액 분사수단16 dead zone 17 caustic soda solution injection means
17a : 밸브 18 : 슬러리 공급부17a: valve 18: slurry supply
본 발명은 필터를 사용하여 슬러리로부터 결정을 회수하는 장치에 있어서, 정제 유기산을 제조하는 과정에서 발생되는 입도가 작은 결정이 필터의 여과매체를 막아 그 기능을 방해하는 것을 방지하기 위한 개량된 구조의 결정회수용 회전진공필터(RVF)에 관한 것이다.The present invention relates to an apparatus for recovering crystals from a slurry using a filter, wherein the crystal structure of the refined organic acid has an improved structure for preventing the small-size crystals from blocking the filter medium of the filter and impairing its function. The present invention relates to a crystal vacuum rotary vacuum filter (RVF).
필터를 사용하여 슬러리로부터 유기산 결정을 회수하는 경우, 유기산 결정에 의해 여과매체의 막힘이 발생한다. 따라서, 종래에는 필터커버를 해체하고 고압수(Water Jet)를 사용하여 세척하거나 새 여과매체로 갈아 끼우거나 하였다. 그러나, 이러한 방법으로 세척하는 경우 세척시간이 오래 걸리고 고압수에 대한 작업자의 위험이 있으며, 미세한 유기산 분말의 비산으로 작업의 애로 및 안전상의 문제 소지가 있고, 고압수 제조를 위한 동력비 및 장치비 그리고 장기간 필터를 사용하지 못함에 따른 경제적 손실이 커지게 된다. 또한, 이러한 방법은 청소를 위한 회전진공필터 운전 정지에서 청소후에 운전 재개까지 장시간(약 18~36시간)이 소요된다.When organic acid crystals are recovered from the slurry using a filter, clogging of the filter medium occurs due to the organic acid crystals. Therefore, conventionally, the filter cover was dismantled and washed using high pressure water (Water Jet) or replaced with a new filter medium. However, when washing in this way, it takes a long time to wash and there is a danger of worker to high pressure water, there is a problem of work and safety problems due to the scattering of fine organic acid powder, power costs and equipment costs for the production of high pressure water and a long time The economic loss of not using a filter increases. In addition, this method takes a long time (about 18 to 36 hours) from the stop of the rotary vacuum filter for cleaning to restarting the operation after cleaning.
따라서, 본 발명의 목적은 상기 문제점을 해결하기 위하여 필터를 사용하여 슬러리로부터 유기산 결정을 회수함에 있어서, 여과매체의 막힘 발생시 여과매체의 교환이나, 고압수의 사용없이 간단한 조작으로 여과 매체를 재사용가능하게 하는 개량된 구조의 결정회수용 회전진공필터를 제공하는데 있다.Accordingly, an object of the present invention is to recover the organic acid crystals from the slurry using a filter in order to solve the above problems, it is possible to reuse the filter medium by simple operation without exchange of the filter medium or the use of high pressure water when clogging of the filter medium occurs. To provide a recovery vacuum rotary vacuum filter having an improved structure.
상기한 목적을 달성하기 위한 본 발명에 의하면, 여과매체의 케이크 제거 영역과 여과영역 사이에 데드존(dead zone)이 존재하며, 여과매체의 상부에 케이크를 세정하는 세정액분사수단이 설치되는, 슬러리로부터 결정을 회수하기 위한 회전진공필터에 있어서, 여과매체 외부에서 여과매체를 세척하기 위한 가성소다 수용액 분사수단이 설치되고, 세정액분사수단에 연결되는 세정액 공급라인이 세정액 공급라인과 순수 공급 라인으로 분리되며, 각각의 공급라인에 밸브가 설치되는 것을 특징으로 하는 슬러리로부터 결정을 회수하기 위한 회전진공필터가 제공된다.According to the present invention for achieving the above object, there is a dead zone between the cake removal region and the filtration region of the filter medium, the slurry is provided with a cleaning liquid spraying means for cleaning the cake on top of the filter medium In the rotary vacuum filter for recovering the crystals from the filter medium, a caustic soda solution injection means for washing the filter medium outside the filter medium is provided, and the cleaning solution supply line connected to the cleaning solution injection means is separated into the cleaning solution supply line and the pure water supply line. In addition, there is provided a rotary vacuum filter for recovering the crystal from the slurry, characterized in that the valve is provided in each supply line.
이하, 본 발명을 더욱 상세히 설명하면 다음과 같다.Hereinafter, the present invention will be described in more detail.
회전진공필터에 의해서 결정을 회수할때, 여과매체의 막힘이 발생되는 원인을 조사한 결과, 필터드럼 내부로의 흡인에 의해 슬러리의 온도가 저하되어, 모액의 과포화에 의해 용질(결정)이 여과매체의 표면에 석출되고, 슬러리의 점도가 높아지는 것 때문인 것으로 알려져 있다.As a result of investigating the cause of clogging of the filter medium when recovering the crystal by the rotary vacuum filter, the temperature of the slurry is lowered by suction into the filter drum, and the solute (crystal) is formed by the supersaturation of the mother liquid. It is known that it is because it precipitates on the surface of and a viscosity of a slurry becomes high.
본 발명에 의하면, 회전진공필터에 테레프탈산 슬러리를 공급하여 원통형의 여과매체를 회전시켜서 흡인여과, 세정, 흡인 여과를 행하여, 슬러리로부터 결정을 회수하는 장치에 있어서, 회전진공필터의 여과매체가 막혔을때, 새로운 여과매체의 교환이나, 고압수를 사용한 세척없이 여과매체를 막은 테레프탈산을 화학적인 방법으로 세척, 제거하여 재사용되도록 설계된다.According to the present invention, there is provided an apparatus for supplying a terephthalic acid slurry to a rotary vacuum filter, rotating a cylindrical filter medium to perform suction filtration, washing, and suction filtration to recover crystals from the slurry, when the filter medium of the rotary vacuum filter is clogged. It is designed to be reused by chemically cleaning and removing terephthalic acid, which is blocked by the filter media, without replacing the new filter media or washing with high pressure water.
본 발명에서는 스러리를 여과할때 여과매체가 결정들로 막히게 되는 점을 해결하기 위해서 상기 결정들을 용해할 수 있는 화학물질을 사용하여 세척함으로써 그 시간을 단축하였는데, 그 화학물질은 테레프탈산 등과 같은 유기산만을 용해할 수 있는 물질로 장치에 부식을 가져오지 않는 것이면 다 적용할 수 있는 바, 특히 본 발명에서는 현재 경제적으로 유리한 가성소다를 이용한다. 가성소다 수용액의 농도는 1~20%가 적당하다. 이러한 농도에서 가성소다 수용액에 테레프탈산 등과 같은 유기산이 순간적으로 녹으므로 세척시간은 매우 짧게 된다. 이때, 농도범위가 이에 미달할 시는 그 효과가 미약하고 이 범위를 초과할 시는 장치에 부식을 가져올 우려가 있어 부적합하다.In the present invention, in order to solve the problem that the filter medium is clogged with crystals when filtering the slurry, the time was shortened by washing with a chemical capable of dissolving the crystals, and the chemical is an organic acid such as terephthalic acid. Any material capable of dissolving the bay can be applied as long as it does not bring corrosion to the apparatus. In particular, the present invention uses caustic soda that is currently economically advantageous. The concentration of the caustic soda solution is preferably 1 to 20%. At such a concentration, since the organic acid such as terephthalic acid is dissolved in an aqueous solution of caustic soda, the washing time is very short. At this time, when the concentration range is less than this, the effect is insignificant, and when the concentration range is exceeded, there is a risk of causing corrosion to the device, which is not suitable.
또한, 본 발명의 회전진공필터에서 가성소다 수용액 분사수단은 여과매체의 케이크 제거 영역과 여과영역 사이에 존재하는 데드존에 설치하는 것이 용이하고 세척에 효과적이어서 바람직하다.In addition, the caustic soda solution injection means in the rotary vacuum filter of the present invention is preferable because it is easy to install in the dead zone existing between the cake removal region and the filtration region of the filter medium and effective for cleaning.
이하, 본 발명을 도면을 참조하여 구체적으로 설명하면 다음과 같다.Hereinafter, the present invention will be described in detail with reference to the drawings.
통상적인 결정회수 장치에, 결정은 슬러리 저장조(21)에 저장된 슬러리(4)를 펌프(23)에 의해 회전진공필터(1)의 하부에 공급하고, 여과매체(3)을 회전시키면서 순차적으로 흡인 여과, 세정, 흡인탈액, 세정된 케이크의 제거에 의해서 회수된다.In a conventional crystal recovery apparatus, the crystals are supplied to the lower portion of the rotary vacuum filter 1 by the pump 23 by the slurry 4 stored in the slurry reservoir 21, and suctioned sequentially while rotating the filter medium 3. It is recovered by filtration, washing, suction stripping and removal of the washed cake.
회전진공필터(1)는 케이싱(2) 내에 횡원통형 여과매체(3)가 자유로이 회전될 수 있게 설치된다. 여과매체(3)의 하부는 케이싱(2) 하부 내측에 형성된 슬러리 섬프(4)에 침지되어 여과영역(5)을 형성하며, 그 내측에는 축적된 세정 및 여과액(6)과 내부가스(7)를 흡인하는 흡인부(8)가 형성되어 있다. 여과매체(3)의 상부에 케이크(9)를 세정하는 세정액분사수단(10)이 설치되어 있고, 이에 대응하는 여과매체(3)는 세정영역(11) 및 그 전후방에 탈액영역(12)을 갖는다. 여과매체(3)의 전방 및 그 내측에는 케이크(9)를 제거하는 블로우부(blow horn)(13) 및 가스 밀폐부(13a)가 설치되어 있으며, 이에 대응하는 여과매체의 부분은 케이크 제거영역(14)이 되며, 그 내측에는 질소 가스 등의 블로우용 가스를 공급하는 가스공급부(15)가 형성되어 있다. 도면부호 18은 슬러리 공급부, 19는 슬러리 순환부, 20은 케이크 취출부, 21은 슬러리 저장조이다. 슬러리(4)는 펌프(22)에 의해 회전진공필터(1)의 슬러리 공급부(18)에 공급되고, 슬러리 순환부(19)를 통해 순환된다. 도면부호 23은 펌프(22)에서 공급된 슬러리(4)의 순환 밸브이며, 24는 슬러리 순환부(19)에서 슬러리 저장조(21)로 슬러리를 회수하는 밸브이다. 28은 세정 및 여과배액조이며, 흡인부(8)로부터 흡인되는 세정 및 여과액(6)과 가스(7)를 입수하여, 펌프(29)에 의해 세정 및 여과액(6)을 배출한다. 30은 세정 및 여과액조(28)의 액면을 일정히 유지하는 조절밸브이다. 여과 및 세정배액조(28)의 가스는 콘덴서(31)를 통해 응축되어 배출된다. 콘덴서에서 분리된 가스는 압축기(32)에 의해 압축된 후 드레인 분리기(33)에서 응축된 분리액은 계외로 배출되고, 응축된 가스는 회전진공필터(1)의 블로우용 가스공급부(15)에 블로우용 가스로 공급된다. 38은 회전진공필터 케이싱(2)내부와 세정 및 여과배액조(28)의 압력 차이를 감지하는 압력계(38)이고, 39는 그 압력차이를 조절하기 위한 조절밸브이다. 40은 건조기로서, 이는 케이크 취출부(20)로부터 취출되는 케이크(9)를 건조하며, 정제된 결정(제품)으로서 취출되도록 한다.The rotary vacuum filter 1 is installed in the casing 2 so that the transverse cylindrical filter medium 3 can be freely rotated. The lower part of the filter medium 3 is immersed in the slurry sump 4 formed inside the casing 2 lower part to form the filtration area 5, and inside the accumulated washing and filtrate 6 and the internal gas 7. The suction part 8 which suctions () is formed. The washing liquid spraying means 10 for washing the cake 9 is provided on the upper portion of the filtering medium 3, and the filtering medium 3 corresponding thereto is provided with the dewatering region 12 in the washing region 11 and before and after. Have A blow horn 13 and a gas seal 13a for removing the cake 9 are provided at the front and the inside of the filter medium 3, and a portion of the filter medium corresponding thereto is a cake removal area. (14), and a gas supply unit 15 for supplying a blow gas such as nitrogen gas is formed therein. Reference numeral 18 is a slurry supply part, 19 is a slurry circulation part, 20 is a cake extraction part, and 21 is a slurry storage tank. The slurry 4 is supplied to the slurry supply part 18 of the rotary vacuum filter 1 by the pump 22, and circulated through the slurry circulation part 19. As shown in FIG. Reference numeral 23 denotes a circulation valve of the slurry 4 supplied from the pump 22, and 24 denotes a valve for recovering the slurry from the slurry circulation unit 19 to the slurry storage tank 21. 28 is a washing | cleaning and filtration drainage tank, the washing | cleaning and filtrate 6 and the gas 7 which are attracted from the suction part 8 are acquired, and the washing | cleaning and filtrate 6 are discharged by the pump 29. FIG. 30 is a control valve for keeping the liquid level of the washing and filtrate tank 28 constant. The gas in the filtration and washing drainage tank 28 is condensed and discharged through the condenser 31. After the gas separated from the condenser is compressed by the compressor 32, the condensate from the drain separator 33 is discharged out of the system, and the condensed gas is supplied to the blow gas supply unit 15 of the rotary vacuum filter 1. It is supplied with blow gas. 38 is a pressure gauge 38 for detecting a pressure difference between the inside of the rotary vacuum filter casing 2 and the cleaning and filtration drainage tank 28, and 39 is a control valve for adjusting the pressure difference. 40 is a dryer, which dries the cake 9 taken out from the cake takeout section 20 and is taken out as purified crystals (products).
상기한 바와같은 회전진공필터(1)에서 본 발명에 따라 여과매체를 세척하기 위하여 개량된 구조에 대하여 설명하기로 한다.The improved structure for washing the filter medium according to the present invention in the rotary vacuum filter 1 as described above will be described.
회전진공필터(1)를 장기간 사용하면 여과액(6)에 과포화된 결정들이 석출하여 여과매체(3)에 달라 붙게되고, 세정액분사수단(10)에 의한 세정 및 블로우용 가스에 의해서도 제거되지 않으므로 여과매체(3)가 막히게 되어 회전진공필터(1)의 효율이 저하된다.When the rotary vacuum filter 1 is used for a long time, crystals supersaturated in the filtrate 6 precipitate and adhere to the filter medium 3, and are not removed even by the gas for cleaning and blow by the washing liquid spraying means 10. The filter medium 3 is blocked and the efficiency of the rotary vacuum filter 1 is lowered.
도시되는 본 발명의 바람직한 실시예에 의하면 회전진공필터(1)에서 케이크 제거 영역(14)과 여과영역(5) 사이에 존재하는 데드존(16)에 가성소다 수용액 분사수단(17)이 설치되고, 세정액분사수단(10)에 연결되는 세정액 공급라인이 세정액 공급라인(10a)과 슈수 공급라인(10b)으로 분리되며, 각각의 공급라인에 밸브가 설치된다.According to a preferred embodiment of the present invention shown in the rotary vacuum filter (1) caustic soda solution injection means 17 is installed in the dead zone 16 existing between the cake removal region 14 and the filtration region (5) The cleaning solution supply line connected to the cleaning solution injection means 10 is separated into the cleaning solution supply line 10a and the water supply line 10b, and valves are provided in the respective supply lines.
상기한 구조의 회전진공필터에서 본 발명에 따라 여과매체를 세척하는 방법에 대해서 설명하면 다음과 같다.Referring to the method of washing the filter medium according to the present invention in the rotary vacuum filter of the above structure as follows.
여과매체의 표면이 결정들로 막혀있을때 필터의 결정회수조작을 중단하고 세척조작을 개시한다. 세척조작은 우선 슬러리 저장조(21)로부터 공급되는 슬러리를 밸브(26)를 잠깐 차단하고 회전진공필터(1)의 슬러리 섬프(4) 및 슬러리 순환부(19)에 있는 슬러리를 모두 배출한 후 세정액을 차단하고, 압축기(32)를 꺼서 블로우용 가스공급을 차단하며, 밸브(17a)를 열어 데드존(16)에 위치하는 가성소다액 분사수단(17)으로 1~20중량%의 가성소다 수용액을 10~100kg/분의 유량으로 분사시킴과 동시에 여과매체를 회전하여 세척한다. 가성소다 세척시간은 2~30분, 바람직하게는 5~15분간 세척한다.When the surface of the filter medium is clogged with crystals, the crystal recovery operation of the filter is stopped and the washing operation is started. In the washing operation, first, the slurry supplied from the slurry reservoir 21 is temporarily blocked by the valve 26, and all the slurry in the slurry sump 4 and the slurry circulation unit 19 of the rotary vacuum filter 1 is discharged, and then the cleaning liquid is discharged. 1 to 20% by weight of caustic soda solution by means of caustic soda solution injection means 17 located in the dead zone 16 by shutting off the compressor 32 and turning off the compressor 32 to block the blow gas supply. While spraying at a flow rate of 10 ~ 100kg / min and at the same time wash the filter media by rotating. Caustic soda washing time is 2 to 30 minutes, preferably 5 to 15 minutes.
가성소다 세척후 세정액분사수단(10)에 연결된 세정액공급라인(10a)의 밸브를 잠그고 순수 공급라인(10b)의 밸브를 열어서 순수를 50~200kg/분의 유량으로 5~30분간, 바람직하게는 70~150kg/분의 유량으로 10~15분간 여과매체(3) 및 회전진공필터(1)의 케이싱(2)에 묻은 가성소다 수용액을 씻어낸다. 이때 슬러리 섬프(4) 및 슬러리 순환부(19)의 드레인 밸브(25)(27)를 열어 가성 소다 수용액 및 순수를 계외로 배출한다.After washing the caustic soda, the valve of the washing liquid supply line 10a connected to the washing liquid spraying means 10 is closed and the valve of the pure water supply line 10b is opened to purify the pure water at a flow rate of 50 to 200 kg / min for 5 to 30 minutes, preferably. The caustic soda solution rinsed in the filter medium 3 and the casing 2 of the rotary vacuum filter 1 is washed for 10 to 15 minutes at a flow rate of 70 to 150 kg / min. At this time, drain valves 25 and 27 of the slurry sump 4 and the slurry circulation part 19 are opened, and caustic soda aqueous solution and pure water are discharged out of the system.
이와같은 본 발명에 의하면 회전진공필터 운전 정지에서 운전 재개까지 1~2시간 소요되므로 획기적인 시간 단축이 가능하다.According to the present invention as described above it takes 1 to 2 hours from stop the operation of the rotary vacuum filter, it is possible to significantly shorten the time.
본 발명을 주로 회전진공필터에 대해서 설명되고 있으나, 당분야의 통상의 지식을 가진자라면 가성소다 수용액과 화학적으로 반응하여 용해될 수 있는 모든 유기산, 특히 테레프탈산, 이소프탈산 및 트리멜리트산 등의 여과에 여과매체를 사용하여 결정을 회수하는 모든 종류의 필터, 예를 들면 배치 및 연속식의 회전가압필터, 디스트필터 및 수평필터 등에도 용이하게 적용할 수 있으며, 이러한 수정 및 변경은 본 발명의 영역에 포함됨은 물론이다.Although the present invention has been described mainly with respect to rotary vacuum filters, those skilled in the art can filter all organic acids, particularly terephthalic acid, isophthalic acid and trimellitic acid, which can be dissolved by chemical reaction with aqueous sodium hydroxide solution. The filter medium can be easily applied to all kinds of filters for recovering crystals, for example, batch and continuous rotary press filters, disc filters, horizontal filters, and the like. Such modifications and variations are within the scope of the present invention. Of course included.
Claims (3)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR1019930032159A KR970004909B1 (en) | 1993-12-31 | 1993-12-31 | Rotary vacuum filter to recover crystals from slurry |
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| Application Number | Priority Date | Filing Date | Title |
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| KR1019930032159A KR970004909B1 (en) | 1993-12-31 | 1993-12-31 | Rotary vacuum filter to recover crystals from slurry |
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| Publication Number | Publication Date |
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| KR950016827A KR950016827A (en) | 1995-07-20 |
| KR970004909B1 true KR970004909B1 (en) | 1997-04-08 |
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| KR1019930032159A Expired - Fee Related KR970004909B1 (en) | 1993-12-31 | 1993-12-31 | Rotary vacuum filter to recover crystals from slurry |
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| KR100493136B1 (en) * | 2002-04-06 | 2005-06-01 | 주식회사 부림이앤씨 | Method for treating waste water from loss-in-quantity process of polyester-based textures |
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