IP Library Granted Patent US 8,558,035
Granted Patent B2
US 8,558,035 · App. 13/148,760 · Granted Oct 15, 2013

Reaction process utilizing critical water

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Quick Facts
Patent No.
US 8,558,035
App. No.
13/148,760
Granted
Oct 15, 2013
Kind
B2
Abstract

In order to perform organic synthesis process through action with supercritical water and acid stably while suppressing a trouble caused by a by-product, a method and an apparatus are provided, including the following steps. Water is supplied to high-pressure pumps ( 110 ) and ( 210 ) from water headers ( 101 ) and ( 201 ), and a pressure-reducing valve ( 324 ) is regulated to increase the pressure to 35 MPa. Temperatures of preheaters ( 120 ) and ( 220 ) and a heater ( 310 ) are increased until the reaction solution is at a temperature of 400° C. Acid (sulfuric acid) and an organic compound raw material (glycerin) are supplied from an acid header ( 203 ) and a raw-material header ( 203 ′) for action with the supercritical water to obtain a reaction solution. The obtained reaction solution is cooled to 100 to 200° C. by first cooling ( 420 ) and a solid component included in the reaction solution is separated for removal from the reaction solution by a filter ( 320 ), and then the reaction solution is cooled to a temperature of about 100° C. or lower by second cooling ( 620 ) and pressure thereof is reduced ( 324 ). Further, the reaction solution is cooled by third cooling ( 720 ) and then a synthesized product (acrolein) is captured.

Claims (35)

1. A method for synthesizing organic matter comprising the steps of:

cooling a reaction solution to 100 to 200° C. by first cooling, the reaction solution being obtained through action of supercritical water and acid with an organic compound raw material;

separating, from the reaction solution, a solid component included in the reaction solution for removal; and

then after cooling the reaction solution to a temperature of about 100° C. or lower by second cooling, reducing pressure.

2. The method for synthesizing organic matter according to claim 1 , wherein after reducing pressure, the reaction solution undergoes third cooling.

3. The method for synthesizing organic matter according to claim 1 , wherein, in the first cooling, cooling water is directly mixed with the reaction solution for cooling.

4. The method for synthesizing organic matter according to claim 2 , wherein the reaction solution after the first cooling includes a material with viscosity of about 0.1 Pa·s or less, the reaction solution after the second cooling includes a material with viscosity of about 10 Pa·s or less, and the reaction solution is cooled by the third cooling to a temperature of a boiling point of a target reaction material or higher.

5. The method for synthesizing organic matter according to claim 2 , wherein a temperature in the third cooling is about 53° C. or higher.

6. The method for synthesizing organic matter according to claim 1 , wherein process from reaction to separation for removal is performed in a vertical pipe separated by a valve.

7. The method for synthesizing organic matter according to claim 1 , wherein process from reaction to separation for removal is performed in a plurality of systems of vertical pipes each separated by a valve.

8. The method for synthesizing organic matter according to claim 1 , wherein the organic compound raw material comprises glycerin and the target reaction material comprises acrolein.

9. An apparatus that synthesizes organic matter, comprising a reactor including: a high-pressure pump for feeding at least water; a preheater for heating the fed water to generate supercritical water; a high-pressure pump for feeding a mixed solution with an organic compound raw material and acid; a preheater for pre-heating the fed mixed solution; a heater for keeping a reaction solution at a reaction temperature, the reaction solution being obtained by mixing the supercritical water with the mixed solution; and a pressure-reducing valve, wherein

along a flow path of the reaction solution, a first cooler, a separation and removal device for solid matters, a second cooler, and a pressure-reducing valve are provided in this order to allow the reaction solution to pass therethrough and be discharged.

10. The apparatus that synthesizes organic matter according to claim 9 , wherein a plurality of systems, each including the first cooler, the separation and removal device for solid matter, the second cooler, and the pressure-reducing valve, are provided in parallel.

11. The method for synthesizing organic matter according to claim 2 , wherein, in the first cooling, cooling water is directly mixed with the reaction solution for cooling.

12. The method for synthesizing organic matter according to claim 11 , wherein the reaction solution after the first cooling includes a material with viscosity of about 0.1 Pa·s or less, the reaction solution after the second cooling includes a material with viscosity of about 10 Pa·s or less, and the reaction solution is cooled by the third cooling to a temperature of a boiling point of a target reaction material or higher.

13. The method for synthesizing organic matter according to claim 3 , wherein the reaction solution after the first cooling includes a material with viscosity of about 0.1 Pa·s or less, the reaction solution after the second cooling includes a material with viscosity of about 10 Pa·s or less, and the reaction solution is cooled by the third cooling to a temperature of a boiling point of a target reaction material or higher.

14. The method for synthesizing organic matter according to claim 3 , wherein a temperature in the third cooling is about 53° C. or higher.

15. The method for synthesizing organic matter according to claim 4 , wherein a temperature in the third cooling is about 53° C. or higher.

16. The method for synthesizing organic matter according to claim 11 , wherein a temperature in the third cooling is about 53° C. or higher.

17. The method for synthesizing organic matter according to claim 2 , wherein process from reaction to separation for removal is performed in a vertical pipe separated by a valve.

18. The method for synthesizing organic matter according to claim 3 , wherein process from reaction to separation for removal is performed in a vertical pipe separated by a valve.

19. The method for synthesizing organic matter according to claim 4 , wherein process from reaction to separation for removal is performed in a vertical pipe separated by a valve.

20. The method for synthesizing organic matter according to claim 5 , wherein process from reaction to separation for removal is performed in a vertical pipe separated by a valve.

21. The method for synthesizing organic matter according to claim 2 , wherein process from reaction to separation for removal is performed in a plurality of systems of vertical pipes each separated by a valve.

22. The method for synthesizing organic matter according to claim 3 , wherein process from reaction to separation for removal is performed in a plurality of systems of vertical pipes each separated by a valve.

23. The method for synthesizing organic matter according to claim 4 , wherein process from reaction to separation for removal is performed in a plurality of systems of vertical pipes each separated by a valve.

24. The method for synthesizing organic matter according to claim 5 , wherein process from reaction to separation for removal is performed in a plurality of systems of vertical pipes each separated by a valve.

25. The method for synthesizing organic matter according to claim 2 , wherein the organic compound raw material comprises glycerin and the target reaction material comprises acrolein.

26. The method for synthesizing organic matter according to claim 3 , wherein the organic compound raw material comprises glycerin and the target reaction material comprises acrolein.

27. The method for synthesizing organic matter according to claim 4 , wherein the organic compound raw material comprises glycerin and the target reaction material comprises acrolein.

28. The method for synthesizing organic matter according to claim 5 , wherein the organic compound raw material comprises glycerin and the target reaction material comprises acrolein.

29. The method for synthesizing organic matter according to claim 6 , wherein the organic compound raw material comprises glycerin and the target reaction material comprises acrolein.

30. The method for synthesizing organic matter according to claim 7 , wherein the organic compound raw material comprises glycerin and the target reaction material comprises acrolein.

31. The apparatus that synthesizes organic matter according to claim 9 , wherein the first cooler is configured to cool the reaction solution to a temperature of 100 to 200° C., and the second cooler is configured to cool the reaction solution to a temperature of about 100° C. or lower.

Assignments (2)
MERGER Recorded Mar 4, 2014
From: HITACHI PLANT TECHNOLOGIES, LTD.
To: HITACHI, LTD.
Reel/Frame 032384/0877 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Aug 10, 2011
From: KONDO, TAKEYUKI; ITO, HIROYUKI; OKAMOTO, NARUYASU; SASE, YASUNARI; MATSUO, TOSHIAKI; OKA, KENICHIRO; KAMIKAWA, MASAYUKI
To: HITACHI PLANT TECHNOLOGIES, LTD.
Reel/Frame 026728/0391 →